Delivery particle

ABSTRACT

The present application relates to encapsulated benefit agents, compositions comprising such encapsulated benefit agents and processes for making and using compositions comprising such encapsulated benefit agents that do not require or require a reduced amount of scavenger materials. Such encapsulated benefit agents, compositions comprising such encapsulated benefit agents are processed such that no or lower levels of scavenger materials are required.

FIELD OF INVENTION

The present application relates to encapsulated benefit agents,compositions comprising such encapsulated benefit agents and processesfor making and using compositions comprising such encapsulated benefitagents.

BACKGROUND OF THE INVENTION

Benefit agents, such as perfumes, silicones, waxes, flavors, vitaminsand fabric softening agents, are expensive and generally less effectivewhen employed at high levels in personal care compositions, cleaningcompositions, and fabric care compositions. As a result, there is adesire to maximize the effectiveness of such benefit agents. One methodof achieving this objective is to improve the delivery efficiencies ofsuch benefit agents. Unfortunately, it is difficult to improve thedelivery efficiencies of benefit agents as such agents may be lost do tothe agents' physical or chemical characteristics, or such agents may beincompatible with other compositional components or the situs that istreated.

In an effort to improve the delivery efficiencies of benefit agents, theindustry, in many cases, encapsulated such benefit agents.Unfortunately, compositions such as melamine formaldehyde microcapsuleslurries may contain materials such as residual formaldehyde that, todate, are removed by introducing scavenger materials into the slurryand/or products containing the aforementioned slurry. While suchmanagement efforts may be effective, such efforts increase formulationcomplexity as scavenger materials can be incompatible with many rawmaterials that are required to formulate a consumer desired product.

Accordingly, there is a need for encapsulated benefit agents,compositions, that do not require or require a reduced level ofscavenger materials, and which comprise such encapsulated benefit agentsand processes for making and using compositions comprising suchencapsulated benefit agents.

SUMMARY OF THE INVENTION

The present application relates to encapsulated benefit agents,compositions comprising such encapsulated benefit agents and processesfor making and using compositions comprising such encapsulated benefitagents that do not require or require reduced amounts of scavengermaterials.

DETAILED DESCRIPTION OF THE INVENTION Definitions

As used herein “consumer product” means baby care, beauty care, fabric &home care, family care, feminine care, health care, snack and/orbeverage products or devices intended to be used or consumed in the formin which it is sold, and not intended for subsequent commercialmanufacture or modification. Such products include but are not limitedto diapers, bibs, wipes; products for and/or methods relating totreating hair (human, dog, and/or cat), including, bleaching, coloring,dyeing, conditioning, shampooing, styling; deodorants andantiperspirants; personal cleansing; cosmetics; skin care includingapplication of creams, lotions, and other topically applied products forconsumer use; and shaving products, products for and/or methods relatingto treating fabrics, hard surfaces and any other surfaces in the area offabric and home care, including: air care, car care, dishwashing, fabricconditioning (including softening), laundry detergency, laundry andrinse additive and/or care, hard surface cleaning and/or treatment, andother cleaning for consumer or institutional use; products and/ormethods relating to bath tissue, facial tissue, paper handkerchiefs,and/or paper towels; tampons, feminine napkins; products and/or methodsrelating to oral care including toothpastes, tooth gels, tooth rinses,denture adhesives, tooth whitening; over-the-counter health careincluding cough and cold remedies, pain relievers, RX pharmaceuticals,pet health and nutrition, and water purification; processed foodproducts intended primarily for consumption between customary meals oras a meal accompaniment (non-limiting examples include potato chips,tortilla chips, popcorn, pretzels, corn chips, cereal bars, vegetablechips or crisps, snack mixes, party mixes, multigrain chips, snackcrackers, cheese snacks, pork rinds, corn snacks, pellet snacks,extruded snacks and bagel chips); and coffee.

As used herein, the term “cleaning composition” includes, unlessotherwise indicated, granular or powder-form all-purpose or “heavy-duty”washing agents, especially cleaning detergents; liquid, gel orpaste-form all-purpose washing agents, especially the so-calledheavy-duty liquid types; liquid fine-fabric detergents; hand dishwashingagents or light duty dishwashing agents, especially those of thehigh-foaming type; machine dishwashing agents, including the varioustablet, granular, liquid and rinse-aid types for household andinstitutional use; liquid cleaning and disinfecting agents, includingantibacterial hand-wash types, cleaning bars, mouthwashes, denturecleaners, dentifrice, car or carpet shampoos, bathroom cleaners; hairshampoos and hair-rinses; shower gels and foam baths and metal cleaners;as well as cleaning auxiliaries such as bleach additives and“stain-stick” or pre-treat types, substrate-laden products such as dryeradded sheets, dry and wetted wipes and pads, nonwoven substrates, andsponges; as well as sprays and mists.

As used herein, the term “fabric care composition” includes, unlessotherwise indicated, fabric softening compositions, fabric enhancingcompositions, fabric freshening compositions and combinations there of.

As used herein, the phrase “benefit agent delivery particle” encompassesmicrocapsules including perfume microcapsules.

As used herein, the terms “particle”, “benefit agent delivery particle”,“capsule” and “microcapsule” are synonymous.

As used herein, the articles including “a” and “an” when used in aclaim, are understood to mean one or more of what is claimed ordescribed.

As used herein, the terms “include”, “includes” and “including” aremeant to be non-limiting.

The test methods disclosed in the Test Methods Section of the presentapplication should be used to determine the respective values of theparameters of Applicants' inventions.

Unless otherwise noted, all component or composition levels are inreference to the active portion of that component or composition, andare exclusive of impurities, for example, residual solvents orby-products, which may be present in commercially available sources ofsuch components or compositions.

All percentages and ratios are calculated by weight unless otherwiseindicated. All percentages and ratios are calculated based on the totalcomposition unless otherwise indicated.

It should be understood that every maximum numerical limitation giventhroughout this specification includes every lower numerical limitation,as if such lower numerical limitations were expressly written herein.Every minimum numerical limitation given throughout this specificationwill include every higher numerical limitation, as if such highernumerical limitations were expressly written herein. Every numericalrange given throughout this specification will include every narrowernumerical range that falls within such broader numerical range, as ifsuch narrower numerical ranges were all expressly written herein.

Benefit Agent Delivery Compositions

Encapsulation processes typically transform two or more monomericmaterials into one or more macromolecules that coat a benefit agent.During the encapsulation process undesirable by-products may be formed.For example, the condensation reaction of amino resins may generateformaldehyde. Attempts to remove such undesirable by-products includethe employment of chemical scavengers. Applicants have surprisinglyfound that even when the residual by-products are managed by theaforementioned chemical means, there is a limit to which suchby-products can be reduced and by-product levels may, over time,increase. Based on such observation, Applicants discovered that theencapsulation process yielded encapsulated benefit agents and shellparticles comprising primarily the aforementioned macromolecules. Inshort, such shell particles may be essentially devoid of benefit agent,yet act as by-product reservoirs. Thus, when such shell particles areremoved, by-product levels may be managed such that dramatically lowerlevels of by-product may be obtained and maintained.

Thus Applicants disclose a benefit agent delivery composition that maycomprise, based on total benefit agent delivery composition weight:

-   -   a.) from about 2% to about 95%, from about 20% to about 75%,        from about 30% to about 70%, or even from about 30% to about        65%, of an encapsulated benefit agent, said encapsulated benefit        agent optionally comprising a sufficient amount of benefit agent        to provide, based on total benefit delivery composition weight        from about 1% to about 85%, from about 8% to about 80%, from        about 12% to about 75%, from about 15% to about 65%, from about        20% to about 60%, or even from about 25% to about 55% benefit        agent;    -   b.) less than from about 1% to about 30%, from about 1% to about        20%, from about 2% to about 20%, from about 5% to about 20%,        from about 5% to about 15%, or even from about 5% to about 12%        shell particles; and    -   c.) the balance of said benefit agent delivery composition being        one or processing aids and/or carriers.

In one aspect of the aforementioned benefit agent delivery compositionsaid encapsulated benefit agent may comprise, a benefit agent selectedfrom the group consisting of perfumes; brighteners; insect repellants;silicones; waxes; flavors; vitamins; fabric softening agents; skin careagents including paraffins; enzymes; anti-bacterial agents; bleaches;and mixtures thereof.

In one aspect of the aforementioned benefit agent delivery compositionsaid shell particles may comprise an amino resin, for example a melamineand/or urea resin.

In one aspect of the aforementioned benefit agent delivery compositionsaid perfume comprises a perfume raw material selected from the groupconsisting of Quadrant I, II, III perfume raw materials and mixturesthereof.

In one aspect of the aforementioned benefit agent delivery compositionsaid one or more processing aids are selected from the group consistingof water, aggregate inhibiting materials such as divalent salts, soilsuspending polymers, and mixtures thereof.

In one aspect of the aforementioned benefit agent delivery compositionsaid one or more carriers may be selected from the group consisting ofpolar solvents, including but not limited to, water, ethylene glycol,propylene glycol, polyethylene glycol, glycerol; nonpolar solvents,including but not limited to, mineral oil, perfume raw materials,silicone oils, hydrocarbon paraffin oils, and mixtures thereof.

In one aspect of the aforementioned benefit agent delivery composition

-   -   a. said perfume may comprise a perfume raw material selected        from the group consisting of Quadrant I, II, III perfume raw        materials and mixtures thereof;    -   b. said one or more processing aids may be selected from the        group consisting of water, aggregate inhibiting materials such        as divalent salts, soil suspending polymers and mixtures        thereof; and    -   c. said one or more carriers may be selected from the group        consisting of water, ethylene glycol, propylene glycol,        polyethylene glycol, glycerol; nonpolar solvents such as mineral        oil, perfume raw materials, silicone oils, hydrocarbon paraffin        oils, and mixtures thereof.

In one aspect, Applicants disclose a benefit agent delivery compositionmade by any of the processes disclosed in the present specification.

Processes of Making Benefit Agent Delivery Compositions

In one aspect, Applicants disclose a process that may comprisesubjecting an benefit agent delivery composition comprising one or moreencapsulated benefit agents and greater than 0.9%, greater than 2.0%,greater than 5%, greater than 10% or even from greater than 10% to about40% shell particles to an operation selected from the group consistingof centrifugation, filtration, solvent exchange, flash evaporation,decantation, flotation separation, spray drying, reactive adsorption,reactive absorption, and combinations thereof, for a sufficient periodof time to reduce the percentage of said shell particles in said benefitagent delivery composition by at least 20%, at least 50%, at least 70%,at least 80%, at least 85%, at least 90%, at least 95% at least 99.9% oreven from about 99.9% to about 99.999%.

In one aspect of the aforementioned process, said centrifugation maycomprise a process selected from the group consisting of:

-   -   a.) batch centrifugation that may comprise applying a        centrifugal force in multiples of gravity of from about 100 to        about 20,000 from about 200 to about 10,000, from about 300 to        about 5,000, from about 500 to about 4,000, from about 1000 to        about 3000 multiples of gravity to said benefit agent delivery        composition, in another aspect, batch centrifugation that may        comprise applying a centrifugal force in multiples of gravity of        from about 100 to about 20,000 from about 200 to about 10,000,        from about 300 to about 9,000, from about 500 to about 8,000,        from about 2,000 to about 7,000 multiples of gravity to said        benefit agent delivery composition;    -   b.) continuous centrifugation that may have at least one of the        following process parameters; a centrifugal force in multiples        of gravity of from about 100 to about 20,000 from about 200 to        about 10,000, from about 300 to about 5,000, from about 500 to        about 4,000, from about 1,000 to about 3,000 multiples of        gravity to said benefit agent delivery composition; an inlet        fluid viscosity of from about 0.1 to about 2000 centipoise, from        about 1 to 500 centipoise, from about 10 to 100 centipoise; an        inlet velocity of the benefit agent delivery composition of from        about 0.2 to about 5 meters per second, from about 0.5 to about        5 meters per second, from about 1 to about 4 meters per second,        or even from about 2 to about 3 meters per second; an the inlet        pressure of the benefit agent delivery composition of from about        10 psig to about 120 psig, from about 20 psig to about 80 psig,        from about 40 psig to about 60 psig; and/or a pressure drop        across the continuous centrifuge, from inlet to outlet, of from        about 3 to about 50 psig, from about 5 to about 40 psig, from        about 10 to about 30 psig, or even from about 10 to about 20        psig; a solids concentration of the benefit agent delivery        composition of from about 0.5 to 90% from about 1 to 50%, from        about 5 to 40% and from about 10 to 35%; in one aspect, said        centrifugal force in multiples of gravity may be from about 100        to about 20,000 from about 200 to about 10,000, from about 300        to about 9,000, from about 500 to about 8,000, from about 2,000        to about 7,000 multiples of gravity to said benefit agent        delivery composition; and    -   c.) combinations thereof

In one aspect of the aforementioned process said continuous processparameters may comprise:

-   -   a.) a centrifugal force in multiples of gravity of from about        100 to about 20,000 from about 200 to about 10,000, from about        300 to about 5,000, from about 500 to about 4,000, from about        1,000 to about 3,000 multiples of gravity to said benefit agent        delivery composition; in another aspect, a centrifugal force may        be in multiples of gravity of from about 100 to about 20,000        from about 200 to about 10,000, from about 300 to about 9,000,        from about 500 to about 8,000, from about 2,000 to about 7,000        multiples of gravity to said benefit agent delivery composition    -   b.) an inlet fluid viscosity of from about 0.1 to about 2000        centipoise, from about 1 to 500 centipoise, from about 10 to 100        centipoise    -   c.) an inlet velocity of the benefit agent delivery composition        of from about 0.2 to about 5 meters per second, from about 0.5        to about 5 meters per second, from about 1 to about 4 meters per        second, or even from about 2 to about 3 meters per second;    -   d.) an the inlet pressure of the benefit agent delivery        composition of from about 10 psig to about 120 psig, from about        20 psig to about 80 psig, from about 40 psig to about 60 psig;    -   e.) a pressure drop across the continuous centrifuge, from inlet        to outlet, of from about 3 to about 50 psig, from about 5 to        about 40 psig, from about 10 to about 30 psig, or even from        about 10 to about 20 psig.

In one aspect of the aforementioned process, said process may comprise afiltration process selected from the group consisting of batchfiltration, continuous filtration and combinations thereof, said processmay comprise at least one of the following process parameters:

-   -   a.) a pressure differential across a filter media, said filter        media having a median pore size is from about 10 kilo Dalton to        about 30 microns, from about 300 kilo Dalton to about 20        microns, from about 0.15 microns to about 18 microns, from about        5 to about 15 microns;    -   b.) a pressure differential across a filter media of from about        5 psig to about 100 psig, from about 10 psig to about 80 psig,        from about 20 psig to about 60 psig, or even from about 30 psig        to about 50 psig;    -   c.) a permeate removal rate of from about 0.1 kg/min/ft² to        about 50 kg/min/ft², from about 0.5 kg/min/ft² to about 30        kg/min/ft², from about 1.0 kg/min/ft² to about 20 kg/min/ft²,        from about 1.5 kg/min/ft² to about 10 kg/min/ft², or even from        about 2 kg/min/ft² to about 5 kg/min/ft².

In one aspect of the aforementioned process, said process may comprisethe following process parameters:

-   -   a.) a pressure differential across a filter media, said filter        media having a median pore size is from about 10 kilo Dalton to        about 30 microns, from about 300 kilo Dalton to about 20        microns, from about 0.15 microns to about 18 microns, from about        5 to about 15 microns;    -   b.) a pressure differential across a filter media of from about        5 psig to about 100 psig, from about 10 psig to about 80 psig,        from about 20 psig to about 60 psig, or even from about 30 psig        to about 50 psig; and    -   c.) a permeate removal rate of from about 0.1 kg/min/ft² to        about 50 kg/min/ft², from about 0.5 kg/min/ft² to about 30        kg/min/ft², from about 1.0 kg/min/ft² to about 20 kg/min/ft²,        from about 1.5 kg/min/ft² to about 10 kg/min/ft², or even from        about 2 kg/min/ft² to about 5 kg/min/ft².

In one aspect of the aforementioned process, said process may comprisedrying said benefit agent delivery composition, said drying may compriseatomizing said benefit agent delivery composition to form benefit agentdelivery composition droplets having a droplet size of from about 2microns to about 200 microns, from about 10 microns to about 150microns, from about 15 microns to about 100 microns, from about 20microns to about 100 microns, from about 30 microns to about 80 microns,from about 50 microns to about 70 microns, said droplets being atomizedin an atomization unit having at least one inlet and one outlet, atleast one of said inlets having an inlet air temperature of from about100° C. to about 280° C., from about 150° C. to about 230° C., fromabout 180° C. to 210° C., or even from about 190° C. to about 200° C.,at least one of said outlets having an outlet air temperature of fromabout 50° C. to about 130° C., from about 70° C. to about 120° C., fromabout 90° C. to about 110° C., or even from about 95° C. to about 105°C.

In one aspect of the aforementioned process, said process may comprise,adsorption and/or absorption that may comprise contacting the benefitagent delivery composition with a adsorption and/or absorption media forfrom about 5 minutes to about 500 minutes, from about 10 minutes toabout 400 minutes, from about 15 minutes to about 300 minutes, fromabout 20 minutes to about 200 minutes, from about 30 minutes to about120 minutes, from about 30 minutes to about 60 minutes; at a benefitagent delivery composition temperature of from about 20° C. to about110° C., from about 30° C. to about 90° C., from about 40° C. to about80° C., from about 50° C. to about 80° C., from about 60° C. to about80° C. and then separating said adsorption and/or absorption media andsaid benefit agent delivery.

In one aspect of the aforementioned process, said process may compriseflotation and/or decantation wherein the benefit agent deliverycomposition is permitted to separate into two or more benefit agentdelivery composition components, one of said components comprising themajority of said shell particles and a second component comprising themajority of said encapsulated benefit agents said second componentcomprising said majority of said encapsulated benefit agent may beseparated from the remainder of said benefit agent delivery components.In one aspect, the phase separation is accelerated by adjusting thedensity of the aqueous phase by the addition of salts (e.g. sodiumchloride, magnesium chloride, calcium chloride, sodium sulfate, and thelike). In one aspect, the phase separation is accelerated by increasingthe temperature of the benefit agent delivery composition. In oneaspect, the phase separation is accelerated by adding more of theaqueous phase, thus causing a dilution of the benefit agent deliverycomposition. In any one or combinations of these aspects of theinvention, said benefit delivery composition is permitted to separatefor a time of from about 0.5 hours to about 96 hours, from about 1 hourto about 72 hours, from about 3 hours to about 48 hours, from about 5hours to about 24 hours, from about 8 hours to about 20 hours, fromabout 10 hours to about 16 hours, or even from about 12 hours to about16 hours.

Applicants also disclose physical processes that may comprise theremoval of a contaminant via desolvation processes, such processesgenerally comprising the steps of (1) addition of a miscible orimmiscible solvent to the benefit agent delivery composition to maximizethe concentration of the contaminant in the solvent phase, (2) removingthe solvent phase containing the high concentration of contaminant, and(3) optionally, reconstituting the solvent-free cake of benefit agentdelivery composition as a means to pass the benefit agent deliverycomposition through one or more additional processes, or alternatively,to improve the properties of the highly concentrated benefit agentdelivery composition such that it is pumpable and handleable. Examplesof processes that comprise these steps include, but are not limited to,centrifugation, filtration, solvent exchange, flash evaporation,decantation, flotation separation, spray drying, reactive adsorption,reactive absorption, electrophoretic separation and combinationsthereof.

In one aspect, batch or continuous centrifugation is utilized to purifythe benefit agent delivery composition. In a batch process, the benefitagent delivery composition is loaded into the centrifuge vessel, andsufficient gravitational force is applied to achieve a phase separation.The centrifugal force measurement that describes the centrifugalacceleration in multiples of gravity, is calculated by the followingequation: w²r/g, the square of the angular velocity (in radians persecond), multiplied by the distance from the center of the centrifuge tothe end of the centrifuge tube (outer surface of the liquid layer, incentimeters), and dividing this by the gravitational force (981centimeters per second, every second). The centrifugal force applied tothe benefit agent delivery composition, in multiples of gravity, is from100 to 20,000 from 200 to 10,000, from 300 to 5,000, from 500 to 4,000,from 1,000 to 3,000 multiples of gravity. In another aspect, thecentrifugal force applied to the benefit agent delivery composition, inmultiples of gravity, may be from 100 to 20,000 from 200 to 10,000, from300 to 9,000, from 500 to 8,000, from 2,000 to 7,000 multiples ofgravity. In a continuous process, the benefit agent delivery compositioncan be pumped into a device that imposes a centrifugal force to thebenefit agent delivery composition. Such processes typically comprise ahigh inlet velocity and a high inlet pressure, and a circular motion ofthe fluid within the device to cause the movement of high densitymaterials to the exterior wall, and lower density materials to thecenter. There are two exit points for the fluid from the device. In thecase of a hydrocyclone, the lower density fluid in the center is removedfrom the device via a tube that extends into the center of the device,the flow rate of this stream is governed by the pressure drop at theexit of the stream. The higher density fluid is removed at the bottom ofthe device, the flow rate of this stream is governed by the pressure atthe exit of the stream.

In the case of a disc stack centrifuge, the machine consists of avertical, rotating bowl with an integral disc stack. The disc stackcontains a set of truncated, conical discs separated by thin spacing orcaulks. The feed is introduced to the rotating bowl in a non-disruptivemanner through the inlet spindle, up to the bottom side of the discstack. Guide ribs are then used to accelerate the slurry to therotational speed of the bowl. Separation occurs in the narrow flowchannel of the disc stack. The heavier solids are thrown outward bycentrifugal force and once they reach the underside of the disc theyslide down along the disc surface. Finally, the solids are thrown to theoutermost position in the bowl where they begin collecting in thesediment holding space. The solids that are collected are continuallyremoved under pressure through a bowl top outlet. The lighter clarifiedliquid moves to the center of the centrifuge and ultimately to the bowltop, where it is also discharged under pressure. The flow rate of bothstreams is governed by the pressure drop across the centrifuge. Bymanipulating the pressure drop across the higher density fluid, one canregulate the % solids and viscosity of the lower density fluid toachieve a continuous separation operation.

The inlet velocity of the benefit agent delivery composition (determinedby dividing the volumetric flow rate of the benefit agent deliverycomposition by the cross-sectional area of the flow tube) can be 0.2 to5 meters per second, from 0.5 to 5 meters per second, from 1 to 4 metersper second, or from 2 to 3 meters per second. The inlet pressure to thehydrocyclone or disc stack centrifuge can be 10 psig to 120 psig, from20 psig to 80 psig, from 40 psig to 60 psig. The bottom of thehydrocyclone is exposed to atmospheric pressure, and this outletcollects the high density particulates and bulk phase. The outletpressure at the top of the cyclone can be manipulated to achieve theright degree of separation of the high density bulk fluid andparticulates from the desired benefit agent delivery particles. In adisc stack centrifuge, the low density fluid phase is collected atatmospheric pressure, whereas the pressure at the higher density fluidphase is manipulated to achieve the desired phase separation.Preferentially, there is at least a pressure difference between theinlet and outlet of the centrifuge, for example a hydrocyclone, of 3 to50 psig, from 5 to 40 psig, from 10 to 30 psig, from 10 to 20 psig.Subsequent dilution of the concentrated benefit agent deliverycomposition can be applied before a second continuous centrifugationcycle. Multiple cycles result in improved purity of the benefit agentdelivery composition. Optionally, the benefit agent delivery compositioncan be diluted with addition of processing materials after the finalcentrifugation cycle, in order to make the benefit agent deliverycomposition shippable, handleable. Such processing materials include,but are not limited to, benefit agent delivery composition dispersingand suspending agent. Such process equipment is available fromAlfa-Lavel (Warminster, Pa., USA), Andritz Bird (Walpole, Mass., USA),Anhydro Inc. (Olympia Fields, Ill., USA), Contec Centrifuges (SanLeandro, Calif., USA), Barrett Centrifugals (Worcester, Mass., USA),Ferrum (Houston, Tex., USA), KMPT USA Inc (Florence, Ky., USA).

In one aspect, the benefit agent delivery composition is purified via afiltration process. The benefit agent delivery composition, optionallydiluted to adjust the flowability of the material, is loaded into apressure filtration unit. The pressure filtration unit contains amembrane through which the benefit agent delivery composition is to befiltered. Such membrane can be a woven or nonwoven material. Woundpolypropylene, polystyrene are examples of woven materials. Spunboundmeltblown polypropylene, or polystyrene are examples of nonwovenmaterials. The membrane median pore size can vary from 10 kilo Dalton to30 microns, from 300 kDa to 20 microns, from 0.15 microns to 18 microns,from 5 to 15 microns. The headspace of the pre-loaded benefit agentdelivery composition is then pressurized with air to a pressure of 5psig to 100 psig, from 10 psig to 80 psig, from 20 psig to 60 psig, from30 psig to 50 psig. The rate of removal of the solvent phase from thebenefit agent delivery composition is monitored. This rate is thendivided by the filter area (total area through which the benefit agentdelivery composition is filtered, i.e. the area over which the membraneis overlaid for filtration). The solvent phase is removed at a permeaterate of 0.1 kg/min/ft2 to 50 kg/min/ft2, from 0.5 to 30 kg/min/ft2, from1.0 to 20 kg/min/ft2, from 1.5 to 10 kg/min/ft2, from 2 to 5 kg/min/ft2.Such process equipment is available from Precision Filtration Products(Pennsburg, Pa., USA), Vacudyne, Inc. (Chicago Heights, Ill., USA),Strainrite Companies (Auburn, Me., USA), Fil-Trek Corporation(Cambridge, Ontario, Canada), Oberlin Filter Co. (Waukesha, Wis., USA).

In one aspect, the benefit agent delivery composition is purified via acontinuous filtration process. The benefit agent delivery composition isoptionally diluted, and continuously pumped through a crossflowfiltration cell. A portion of the solvent phase of the benefit agentdelivery composition is removed through the membrane as permeate. Thefiltration cell comprises a microfiltration or ultrafiltration membrane.The membrane median pore size can vary from 10 kilo Dalton to 30microns, from 300 kDa to 20 microns, from 0.15 microns to 18 microns,from 5 to 15 microns. The transmembrane pressure (the arithmetic averageof the pressures before and after the membrane modulus minus thepermeate pressure) is a function if the benefit agent deliverycomposition flowrate, and can be optimized by determining the pressureat which there is a maximum in the permeate flow rate. The transmembranepressure can be from 5 psig to 150 psig, from 10 psig to 100 psig, from20 psig to 80 psig, from 30 psig to 50 psig. The rate of removal of thesolvent phase from the benefit agent delivery composition is monitored.This rate is then divided by the total filter area. The solvent phase isremoved at a permeate rate of 0.1 kg/min/ft2 to 50 kg/min/ft2, from 0.5to 30 kg/min/ft2, from 1.0 to 20 kg/min/ft2, from 1.5 to 10 kg/min/ft2,from 2 to 5 kg/min/ft2. Such process equipment is available from PallCorporation (East Hills, N.Y., USA), GEA Filtration (Hudson, Wis., USA),and Millipore Corporation (Kankakee, Ill., USA).

In one aspect, the benefit agent delivery composition is purified via aspray drying process. The benefit agent delivery composition isoptionally diluted to achieve the desired flowability of the material.The composition is then atomized through a centrifugal nozzle, apressure nozzle, a two-fluid nozzle, or combinations thereof into adrying chamber. Airflow through the chamber is co-current orcounter-current, preferably co-current at an inlet temperature of 100degrees Centigrade to 280 degrees Centigrade, from 150 to 230 degreesCentigrade, from 180 to 210 degrees Centigrade, from 190 to 200 degreesCentigrade. The benefit agent delivery composition is atomized into adroplet size of 2 microns to 200 microns, from 10 microns to 150microns, from 15 microns to 100 microns, from 20 microns to 100 microns,from 30 microns to 80 microns, from 50 microns to 70 microns. The driedparticles are collected from the spray drying chamber through a cyclone,at an outlet air temperature of from 50 to 130 degrees Centigrade, from70 to 120 degrees Centigrade, from 90 to 110 degrees centigrade, from 95to 105 degrees Centigrade. Such process equipment is available from GEANiro Inc. (Columbia, Md., USA), American Custom Drying (Burlington,N.J., USA), Spray-Tek Inc. (Middlesex, N.J., USA).

In one aspect, the benefit agent delivery composition is purified via adecantation process. The benefit agent delivery composition is placed ina vat, and allowed to age. Optionally, air is allowed to flow throughthe benefit agent delivery composition to increase the rate of phaseseparation. The benefit agent delivery composition is aged for 0.5 hoursto 96 hours, from 1 hour to 72 hours, from 3 hours to 48 hours, from 5hours to 24 hours, from 8 hours to 20 hours, from 10 hours to 16 hours,or even from 12 hours to 16 hours. The phase separated benefit agentdelivery particles are skimmed off from the top of the benefit agentdelivery composition in the vat. Such process equipment is availablefrom Alfa-Lavel Separation (Warminster, Pa., USA), Braodbent (FortWorth, Tex., USA), Centrisys Corporation (Kenosha, Wis., USA), ContecCentrifuges (San Leandro, Calif., USA), Flottweg (Vilsbiburg, Germany),Decanter Machine (Johnson City, Tenn., USA), Jenkins Centrifuge (NorthKansas City, Mo., USA), Pennwalt India (Searing Town, N.Y., USA).

In one aspect, the benefit delivery composition is purified viaelectrophoretic separation. The benefit delivery composition isoptionally diluted and placed in a vessel with anode and cathode plates.In one aspect the anode is positioned near the lower end of thecontainer. The cathode is positioned near the top. A potential isapplied. The shell particles migrate to respective electrodes dependingon polarity of the shell particles. With urea formaldehyde capsulesparticles were seen to migrate to the cathode.

The cathode is generally the electrode through which electric currentflows out of a polarized electrical device, or where reduction occurs.Positively charged cation tend to move toward the cathode, and in thelocation where oxidation occurs. The anode tends to attract anions.Cationic changed particles tend to migrate to the cathode.

For electrophoretic separation, an electrical potential is appliedbetween the electrodes such as with a dry cell or other voltage source.

For example a capsule slurry, at 10% solids can be placed in a beakerusing a copper anode and cathode plate. A 6 volt charge is appliedacross the plates using a 6 volt lantern battery. The capsules are seento migrate to the cathode in as little as twenty minutes.

In an alternate aspect, electrophoretic separation can be used alone orcombined with any of the processes of centrifugation, filtration,solvent exchange, flash evaporation, decantation, flotation separation,spray drying, reactive absorption, reactive adsorption and combinationsthereof.

The capsule slurry was ascertained to have a zeta potential more than60, and therefore generally a stable emulsion. By applying an electricor magnetic field of sufficient potential, the colloidal particles canbe made to coagulate or flocculate at one of the electrodes.

Electrophoretic separation can be applied in a batch or continuousprocess.

Encapsulates

Suitable encapsulates may be made by the teachings herein or purchasedfrom Firmenich (Geneva, Switzerland), Givaudan (Argenteuil, France), IFF(Hazlet, N.J. USA), BASF (Ludwigshafen, Germany), Cognis (Monheim,Germany), Syngenta (Germany), Ciba (Basel, Switzerland), Rhodia Chimie(Lyon, France), Appleton Papers (Appleton, Wis., USA), Aveka(Minneapolis, Minn., USA), R.T. Dodge (Dayton, Ohio, USA). The wallmaterials of useful encapsulates may comprise materials selected fromthe group consisting of polyethylenes, polyamides, polystyrenes,polyisoprenes, polycarbonates, polyesters, polyacrylates, polyureas,polyurethanes, polyolefins, polysaccharides, epoxy resins, vinylpolymers, and mixtures thereof. In one aspect, useful wall materialsinclude materials that are sufficiently impervious to the core materialand the materials in the environment in which the encapsulated benefitagent will be employed, to permit the delivery benefit to be obtained.Suitable impervious wall materials include materials selected from thegroup consisting of reaction products of one or more amines with one ormore aldehydes, such as urea cross-linked with formaldehyde orgluteraldehyde, melamine cross-linked with formaldehyde;gelatin-polyphosphate coacervates optionally cross-linked withgluteraldehyde; gelatin-gum Arabic coacervates; cross-linked siliconefluids; polyamine reacted with polyisocyanates and mixtures thereof. Inone aspect, the wall material comprises melamine cross-linked withformaldehyde.

The core of the encapsulated benefit agent may comprise perfume rawmaterials, silicone oils, waxes, hydrocarbons, higher fatty acids,essential oils, lipids, skin coolants, vitamins, sunscreens,antioxidants, glycerine, catalysts, bleach particles, silicon dioxideparticles, malodor reducing agents, odor-controlling materials,chelating agents, antistatic agents, softening agents, insect and mothrepelling agents, colorants, antioxidants, chelants, bodying agents,drape and form control agents, smoothness agents, wrinkle controlagents, sanitization agents, disinfecting agents, germ control agents,mold control agents, mildew control agents, antiviral agents, dryingagents, stain resistance agents, soil release agents, fabric refreshingagents and freshness extending agents, chlorine bleach odor controlagents, dye fixatives, dye transfer inhibitors, color maintenanceagents, optical brighteners, color restoration/rejuvenation agents,anti-fading agents, whiteness enhancers, anti-abrasion agents, wearresistance agents, fabric integrity agents, anti-wear agents,anti-pilling agents, defoamers and anti-foaming agents, UV protectionagents for fabrics and skin, sun fade inhibitors, anti-allergenicagents, enzymes, water proofing agents, fabric comfort agents, shrinkageresistance agents, stretch resistance agents, stretch recovery agents,skin care agents, glycerin, and natural actives such as aloe vera,vitamin E, shea butter, cocoa butter, and the like, brighteners,antibacterial actives, antiperspirant actives, cationic polymers andmixtures thereof. In one aspect, said perfume raw material is selectedfrom the group consisting of alcohols, ketones, aldehydes, esters,ethers, nitriles alkenes. In one aspect the core material may comprise aperfume. In one aspect, said perfume may comprise perfume raw materialsselected from the group consisting of alcohols, ketones, aldehydes,esters, ethers, nitriles alkenes and mixtures thereof. In one aspect,said perfume may comprise a perfume raw material selected from the groupconsisting of perfume raw materials having a boiling point (B.P.) lowerthan about 250° C. and a ClogP lower than about 3, perfume raw materialshaving a B.P. of greater than about 250° C. and a ClogP of greater thanabout 3, perfume raw materials having a B.P. of greater than about 250°C. and a ClogP lower than about 3, perfume raw materials having a B.P.lower than about 250° C. and a ClogP greater than about 3 and mixturesthereof. Perfume raw materials having a boiling point B.P. lower thanabout 250° C. and a ClogP lower than about 3 are known as Quadrant Iperfume raw materials, perfume raw materials having a B.P. of greaterthan about 250° C. and a ClogP of greater than about 3 are known asQuadrant IV perfume raw materials, perfume raw materials having a B.P.of greater than about 250° C. and a ClogP lower than about 3 are knownas Quadrant II perfume raw materials, perfume raw materials having aB.P. lower than about 250° C. and a ClogP greater than about 3 are knownas a Quadrant III perfume raw materials. In one aspect, said perfumecomprises a perfume raw material having B.P. of lower than about 250° C.In one aspect, said perfume may comprise a perfume raw material selectedfrom the group consisting of Quadrant I, II, III perfume raw materialsand mixtures thereof. In one aspect, said perfume comprises a QuadrantIII perfume raw material. Suitable Quadrant I, II, III and IV perfumeraw materials are disclosed in U.S. Pat. No. 6,869,923 B1.

In one aspect, said perfume may comprise a Quadrant IV perfume rawmaterial. While not being bound by theory, it is believed that suchQuadrant IV perfume raw materials can improve perfume odor “balance”.Said perfume may comprise, based on total perfume weight, less thanabout 30%, less than about 20%, or even less than about 15% of saidQuadrant IV perfume raw material.

The perfume raw materials and accords may be obtained from one or moreof the following companies Firmenich (Geneva, Switzerland), Givaudan(Argenteuil, France), IFF (Hazlet, N.J.), Quest (Mount Olive, N.J.),Bedoukian (Danbury, Conn.), Sigma Aldrich (St. Louis, Mo.), MillenniumSpecialty Chemicals (Olympia Fields, Ill.), Polarone International(Jersey City, N.J.), Fragrance Resources (Keyport, N.J.), and Aroma &Flavor Specialties (Danbury, Conn.).

Process of Making Encapsulated Benefit Agents

The encapsulated benefit agents employed herein may be made via theteachings of U.S. Pat. No. 6,592,990 B2 and/or U.S. Pat. No. 6,544,926B1 and the examples disclosed herein.

Anionic emulsifiers are typically used during the encapsulation processto emulsify the benefit agent prior to microcapsule formation. While notbeing bound by theory, it is believed that the anionic materialsadversely interact with the cationic surfactant actives that are oftenfound in compositions such as fabric care compositions—this may yield anaesthetically unpleasing aggregation of particles that are employed insaid composition. In addition to the unacceptable aesthetics, suchaggregates may result in rapid phase separation of the particles fromthe bulk phase. Applicants discovered that such aggregates can beprevented by the addition of certain aggregate inhibiting materialsincluding materials selected from the group consisting of salts,polymers and mixtures thereof. Useful aggregate inhibiting materialsinclude, divalent salts such as magnesium salts, for example, magnesiumchloride, magnesium acetate, magnesium phosphate, magnesium formate,magnesium bromide, magnesium titanate, magnesium sulfate heptahydrate;calcium salts, for example, calcium chloride, calcium formate, calciumcalcium acetate, calcium bromide; trivalent salts, such as aluminumsalts, for example, aluminum sulfate, aluminum phosphate, aluminumchloride n-hydrate and polymers that have the ability to suspend anionicparticles such as soil suspension polymers, for example, polyethyleneimines, alkoxylated polyethylene imines, polyquaternium-6 andpolyquaternium-7, xanthan gum, gellan gum, carageenan gum, carboxymethylcellulose, and mixtures thereof.

In one aspect of the invention, encapsulated benefit agents aremanufactured and are subsequently coated with a material to reduce therate of leakage of the benefit agent from the particles when theparticles are subjected to a bulk environment containing, for example,surfactants, polymers, and solvents. Non-limiting examples of coatingmaterials that can serve as barrier materials include materials selectedfrom the group consisting of polyvinyl pyrrolidone homopolymer, and itsvarious copolymers with styrene, vinyl acetate, imidazole, primary andsecondary amine containing monomers, methyl acrylate, polyvinyl acetal,maleic anhydride; polyvinyl alcohol homopolymer, and its variouscopolymers with vinyl acetate, 2-acrylamide-2-methylpropane sulfonate,primary and secondary amine containing monomers, imidazoles, methylacrylate; polyacrylamides; polyacrylic acids; microcrystalline waxes;paraffin waxes; modified polysaccharides such as waxy maize or dent cornstarch, octenyl succinated starches, derivatized starches such ashydroxyethylated or hydroxypropylated starches, carrageenan, guar gum,pectin, xanthan gum; modified celluloses such as hydrolyzed celluloseacetate, hydroxy propyl cellulose, methyl cellulose, and the like;modified proteins such as gelatin; hydrogenated and non-hydrogenatedpolyalkenes; fatty acids; hardened shells such as urea crosslinked withformaldehyde, gelatin-polyphosphate, melamine-formaldehyde, polyvinylalcohol crosslinked with sodium tetraborate or gluteraldehyde; latexesof styrene-butadiene, ethyl cellulose, inorganic materials such as claysincluding magnesium silicates, aluminosilicates; sodium silicates, andthe like; and mixtures thereof. Such materials can be obtained from CPKelco Corp. of San Diego, Calif., USA; Degussa AG or Dusseldorf,Germany; BASF AG of Ludwigshafen, Germany; Rhodia Corp. of Cranbury,N.J., USA; Baker Hughes Corp. of Houston, Tex., USA; Hercules Corp. ofWilmington, Del., USA; Agrium Inc. of Calgary, Alberta, Canada, ISP ofNew Jersey U.S.A.

Suitable equipment for use in the processes disclosed herein may includecontinuous stirred tank reactors, homogenizers, turbine agitators,recirculating pumps, paddle mixers, ploughshear mixers, ribbon blenders,vertical axis granulators and drum mixers, both in batch and, whereavailable, in continuous process configurations, spray dryers, andextruders. Such equipment can be obtained from Lodige GmbH (Paderborn,Germany), Littleford Day, Inc. (Florence, Ky., U.S.A.), Forberg AS(Larvik, Norway), Glatt Ingenieurtechnik GmbH (Weimar, Germany), Niro(Soeborg, Denmark), Hosokawa Bepex Corp. (Minneapolis, Minn., USA), ArdeBarinco (New Jersey, USA).

Formaldehyde Scavenging

In one aspect, encapsulated benefit agent may be combined with aformaldehyde scavenger. In one aspect, encapsulated benefit agent maycomprise the encapsulated benefit agent of the present invention.Suitable formaldehyde scavengers include materials selected from thegroup consisting of sodium bisulfate, urea, ethylene urea, cysteine,cysteamine, lysine, glycine, serine, carnosine, histidine, glutathione,3,4-diaminobenzoic acid, allantoin, glycouril, anthranilic acid, methylanthranilate, methyl 4-aminobenzoate, ethyl acetoacetate,acetoacetamide, malonamide, ascorbic acid, 1,3-dihydroxyacetone dimer,biuret, oxamide, benzoguanamine, pyroglutamic acid, pyrogallol, methylgallate, ethyl gallate, propyl gallate, triethanol amine, succinamide,thiabendazole, benzotriazol, triazole, indoline, sulfanilic acid,oxamide, sorbitol, glucose, cellulose, poly(vinyl alcohol), partiallyhydrolyzed poly(vinylformamide), poly(vinyl amine), poly(ethyleneimine), poly(oxyalkyleneamine), poly(vinyl alcohol)-co-poly(vinylamine), poly(4-aminostyrene), poly(l-lysine), chitosan, hexane diol,ethylenediamine-N,N′-bisacetoacetamide, N-(2-ethylhexyl)acetoacetamide,2-benzoylacetoacetamide, N-(3-phenylpropyl)acetoacetamide, lilial,helional, melonal, triplal, 5,5-dimethyl-1,3-cyclohexanedione,2,4-dimethyl-3-cyclohexenecarboxaldehyde,2,2-dimethyl-1,3-dioxan-4,6-dione, 2-pentanone, dibutyl amine,triethylenetetramine, ammonium hydroxide, benzylamine,hydroxycitronellol, cyclohexanone, 2-butanone, pentane dione,dehydroacetic acid, or a mixture thereof. These formaldehyde scavengersmay be obtained from Sigma/Aldrich/Fluka of St. Louis, Mo. U.S.A. orPolySciences, Inc. of Warrington, Pa. U.S.A.

In one aspect, resins that are insoluble in the benefit agent deliverycomposition are surface modified with such formaldehyde scavengers.Typically polymeric beads of 50 microns to 5000 microns, from 100microns to 4500 microns, from 200 microns to 3500 microns, from 500microns to 2000 microns, from 800 microns to 1500 microns are surfacemodified with formaldehyde scavenging materials. Such surface modifiedresins are incorporated into the benefit agent delivery composition andallowed to scavenge formaldehyde. Typically, the benefit agent deliverycomposition temperature is adjusted to 20 to 110 degrees Centigrade,from 30 to 90 degrees Centigrade, from 40 to 80 degrees Centigrade, from50 to 80 degrees Centigrade, from 60 to 80 degrees Centigrade. Suchformaldehyde scavengers are allowed to scavenge formaldehyde from thebenefit agent delivery composition for 5 to 500 minutes, from 10 to 400minutes, from 15 to 300 minutes, from 20 to 200 minutes, from 30 to 120minutes, from 30 to 60 minutes. Subsequently, the insoluble resins areremoved from the benefit agent delivery composition via a filtrationprocess, to yield a polymer resin free benefit agent deliverycomposition. Examples of such resins include, but are not limited to,aminoethylated polystyrene, polymer bound diethylenetriamine, polymerbound p-toluenesulfonylhydrazine. Such materials are available fromAldrich (Milwaukee, Wis., USA). Commercial scavenging resins withtradenames ScavengePore®, Argopore®-NH2-L, JandaJel-NH2, StratospheresPL-AMS are also available from Aldrich (Milwaukee, Wis., USA).

Such formaldehyde scavengers are typically combined with a slurrycontaining said benefit agent delivery particle, at a level, based ontotal slurry weight, of from about 2 wt. % to about 18 wt. %, from about3.5 wt. % to about 14 wt. % or even from about 5 wt. % to about 13 wt.%.

In one aspect, such formaldehyde scavengers may be combined with aproduct containing a benefit agent delivery particle, said scavengersbeing combined with said product at a level, based on total productweight, of from about 0.005% to about 0.8%, alternatively from about0.03% to about 0.5%, alternatively from about 0.065% to about 0.25% ofthe product formulation.

In another aspect, such formaldehyde scavengers may be combined with aslurry containing said encapsulated benefit agent, at a level, based ontotal slurry weight, of from about 2 wt. % to about 14 wt. %, from about3.5 wt. % to about 14 wt. % or even from about 5 wt. % to about 14 wt. %and said slurry may be added to a product matrix to which addition anidentical or different scavenger may be added at a level, based on totalproduct weight, of from about 0.005% to about 0.5%, alternatively fromabout 0.01% to about 0.25%, alternatively from about 0.05% to about0.15% of the product formulation,

In one aspect, one or more of the aforementioned formaldehyde scavengersmay be combined with a consumer product containing an encapsulatedbenefit agent at a level, based on total liquid fabric enhancing productweight, of from 0.005% to about 0.8%, alternatively from about 0.03% toabout 0.4%, alternatively from about 0.06% to about 0.25% of the productformulation

In one aspect, such formaldehyde scavengers may be combined with aliquid laundry detergent product containing a benefit agent deliveryparticle, said scavengers being selected from the group consisting ofsodium bisulfite, urea, ethylene urea, cysteine, cysteamine, lysine,glycine, serine, carnosine, histidine, glutathione, 3,4-diaminobenzoicacid, allantoin, glycouril, anthranilic acid, methyl anthranilate,methyl 4-aminobenzoate, ethyl acetoacetate, acetoacetamide, malonamide,ascorbic acid, 1,3-dihydroxyacetone dimer, biuret, oxamide,benzoguanamine, pyroglutamic acid, pyrogallol, methyl gallate, ethylgallate, propyl gallate, triethanol amine, succinamide, thiabendazole,benzotriazol, triazole, indoline, sulfanilic acid, oxamide, sorbitol,glucose, cellulose, poly(vinyl alcohol), partially hydrolyzedpoly(vinylformamide), poly(vinyl amine), poly(ethylene imine),poly(oxyalkyleneamine), poly(vinyl alcohol)-co-poly(vinyl amine),poly(4-aminostyrene), poly(l-lysine), chitosan, hexane diol,ethylenediamine-N,N′-bisacetoacetamide, N-(2-ethylhexyl)acetoacetamide,2-benzoylacetoacetamide, N-(3-phenylpropyl)acetoacetamide, lilial,helional, melonal, triplal, 5,5-dimethyl-1,3-cyclohexanedione,2,4-dimethyl-3-cyclohexenecarboxaldehyde,2,2-dimethyl-1,3-dioxan-4,6-dione, 2-pentanone, dibutyl amine,triethylenetetramine, ammonium hydroxide, benzylamine,hydroxycitronellol, cyclohexanone, 2-butanone, pentane dione,dehydroacetic acid and mixtures thereof, and combined with said liquidlaundry detergent product at a level, based on total liquid laundrydetergent product weight, of from about 0.003 wt. % to about 0.20 wt. %,from about 0.03 wt. % to about 0.20 wt. % or even from about 0.06 wt. %to about 0.14 wt. %.

In one aspect, such formaldehyde scavengers may be combined with a hairconditioning product containing a benefit agent delivery particle, at alevel, based on total hair conditioning product weight, of from about0.003 wt. % to about 0.30 wt. %, from about 0.03 wt. % to about 0.20 wt.% or even from about 0.06 wt. % to about 0.14 wt. %., said selection ofscavengers being identical to the list of scavengers in the previousparagraph relating to a liquid laundry detergent product.

Compositions Comprising Benefit Agent Delivery Compositions

In one aspect, a consumer product comprising the benefit agent deliverycomposition as described in any of the various aspects of the productset forth herein and a consumer product adjunct is disclosed. In oneaspect, said consumer product adjunct is selected from the groupconsisting of polymers, for example cationic polymers, surfactants,builders, chelating agents, dye transfer inhibiting agents, dispersants,enzymes, and enzyme stabilizers, catalytic materials, bleach activators,polymeric dispersing agents, clay soil removal/anti-redeposition agents,brighteners, suds suppressors, dyes, additional perfume and perfumedelivery systems, structure elasticizing agents, fabric softeners,carriers, hydrotropes, processing aids and/or pigments and mixturesthereof.

In one aspect, said consumer product may comprise, based on totalconsumer product weight, from about 0.1% to about 20%, from about 0.2%to about 15%, from about 0.3% to about 10%, from about 0.4% to about 8%,or even from about 0.5% to about 5% of any of the benefit agent deliverycompositions disclosed in the present specification.

In one aspect, a composition that may comprise any of the benefit agentdelivery compositions of the present specification and a materialselected from the group consisting of dyes; perfume; opticalbrighteners; deposition aids; and mixtures thereof.

In one aspect, a consumer product that may comprise, based on totalconsumer product weight:

-   -   a.) from about 0.1% to about 5%, encapsulated benefit agent,        said benefit agent comprising an amino resin;    -   1. from about 1 ppm to about 150 ppm, from about 1 ppm to about        100 ppm, from about 1 ppm to about 50 ppm formaldehyde or even        from about 1 ppm to about 10 ppm; and    -   2. less than about 0.3 weight %, less than about 0.1 weight %,        less than about 0.01 weight % from less than about 0.01 weight %        to about 0.0001 weight % formaldehyde scavenger based on total        consumer product weight is disclosed.

In one aspect, said consumer products may be a powdered, granule orother essentially dry detergent.

Aspects of the invention include the use of the benefit agent deliverycomposition of the present invention in laundry detergent compositions(e.g., TIDE™), hard surface cleaners (e.g., MR CLEAN™), automaticdishwashing liquids (e.g., CASCADE™), and floor cleaners (e.g.,SWIFFER™). Non-limiting examples of cleaning compositions may includethose described in U.S. Pat. Nos. 4,515,705; 4,537,706; 4,537,707;4,550,862; 4,561,998; 4,597,898; 4,968,451; 5,565,145; 5,929,022;6,294,514; and 6,376,445. The cleaning compositions disclosed herein aretypically formulated such that, during use in aqueous cleaningoperations, the wash water will have a pH of between about 6.5 and about12, or between about 7.5 and 10.5. Liquid dishwashing productformulations typically have a pH between about 6.8 and about 9.0.Cleaning products are typically formulated to have a pH of from about 7to about 12. Techniques for controlling pH at recommended usage levelsinclude the use of buffers, alkalis, acids, etc., and are well known tothose skilled in the art.

Method of Use

In one aspect, a method of treating and/or cleaning a situs, isdisclosed. Said method may comprise optionally washing and/or rinsingsaid situs; contacting said situs with any single or combination ofbenefit agent delivery composition disclosed in the presentspecification; and optionally washing and/or rinsing said situs. In oneaspect, a situs treated in accordance with such method is disclosed.

Adjunct Materials

While not essential for the purposes of the present invention, thenon-limiting list of adjuncts illustrated hereinafter are suitable foruse in the instant compositions and may be desirably incorporated incertain embodiments of the invention, for example to assist or enhanceperformance, for treatment of the substrate to be cleaned, or to modifythe aesthetics of the composition as is the case with perfumes,colorants, dyes or the like. It is understood that such adjuncts are inaddition to the components that are supplied via Applicants'agglomerate/particle. The precise nature of these additional components,and levels of incorporation thereof, will depend on the physical form ofthe composition and the nature of the operation for which it is to beused. Suitable adjunct materials include, but are not limited to,polymers, for example cationic polymers, surfactants, builders,chelating agents, dye transfer inhibiting agents, dispersants, enzymes,and enzyme stabilizers, catalytic materials, bleach activators,polymeric dispersing agents, clay soil removal/anti-redeposition agents,brighteners, suds suppressors, dyes, additional perfume and perfumedelivery systems, structure elasticizing agents, fabric softeners,carriers, hydrotropes, processing aids and/or pigments. In addition tothe disclosure below, suitable examples of such other adjuncts andlevels of use are found in U.S. Pat. Nos. 5,576,282, 6,306,812 B1 and6,326,348 B1 that are incorporated by reference.

As stated, the adjunct ingredients are not essential to Applicants'cleaning and fabric care compositions. Thus, certain embodiments ofApplicants' compositions do not contain one or more of the followingadjuncts materials: bleach activators, surfactants, builders, chelatingagents, dye transfer inhibiting agents, dispersants, enzymes, and enzymestabilizers, catalytic metal complexes, polymeric dispersing agents,clay and soil removal/anti-redeposition agents, brighteners, sudssuppressors, dyes, additional perfumes and perfume delivery systems,structure elasticizing agents, fabric softeners, carriers, hydrotropes,processing aids and/or pigments. However, when one or more adjuncts ispresent, such one or more adjuncts may be present as detailed below:

Surfactants—The compositions according to the present invention cancomprise a surfactant or surfactant system wherein the surfactant can beselected from nonionic and/or anionic and/or cationic surfactants and/orampholytic and/or zwitterionic and/or semi-polar nonionic surfactants.The surfactant is typically present at a level of from about 0.1%, fromabout 1%, or even from about 5% by weight of the cleaning compositionsto about 99.9%, to about 80%, to about 35%, or even to about 30% byweight of the cleaning compositions.

Builders—The compositions of the present invention can comprise one ormore detergent builders or builder systems. When present, thecompositions will typically comprise at least about 1% builder, or fromabout 5% or 10% to about 80%, 50%, or even 30% by weight, of saidbuilder. Builders include, but are not limited to, the alkali metal,ammonium and alkanolammonium salts of polyphosphates, alkali metalsilicates, alkaline earth and alkali metal carbonates, aluminosilicatebuilders polycarboxylate compounds. ether hydroxypolycarboxylates,copolymers of maleic anhydride with ethylene or vinyl methyl ether,1,3,5-trihydroxybenzene-2,4,6-trisulphonic acid, andcarboxymethyl-oxysuccinic acid, the various alkali metal, ammonium andsubstituted ammonium salts of polyacetic acids such as ethylenediaminetetraacetic acid and nitrilotriacetic acid, as well as polycarboxylatessuch as mellitic acid, succinic acid, oxydisuccinic acid, polymaleicacid, benzene 1,3,5-tricarboxylic acid, carboxymethyloxysuccinic acid,and soluble salts thereof.

Chelating Agents—The compositions herein may also optionally contain oneor more copper, iron and/or manganese chelating agents. If utilized,chelating agents will generally comprise from about 0.1% by weight ofthe compositions herein to about 15%, or even from about 3.0% to about15% by weight of the compositions herein.

Dye Transfer Inhibiting Agents—The compositions of the present inventionmay also include one or more dye transfer inhibiting agents. Suitablepolymeric dye transfer inhibiting agents include, but are not limitedto, polyvinylpyrrolidone polymers, polyamine N-oxide polymers,copolymers of N-vinylpyrrolidone and N-vinylimidazole,polyvinyloxazolidones and polyvinylimidazoles or mixtures thereof. Whenpresent in the compositions herein, the dye transfer inhibiting agentsare present at levels from about 0.0001%, from about 0.01%, from about0.05% by weight of the cleaning compositions to about 10%, about 2%, oreven about 1% by weight of the cleaning compositions.

Dispersants—The compositions of the present invention can also containdispersants. Suitable water-soluble organic materials are the homo- orco-polymeric acids or their salts, in which the polycarboxylic acid maycomprise at least two carboxyl radicals separated from each other by notmore than two carbon atoms.

Enzymes—The compositions can comprise one or more detergent enzymeswhich provide cleaning performance and/or fabric care benefits. Examplesof suitable enzymes include, but are not limited to, hemicellulases,peroxidases, proteases, cellulases, xylanases, lipases, phospholipases,esterases, cutinases, pectinases, keratanases, reductases, oxidases,phenoloxidases, lipoxygenases, ligninases, pullulanases, tannases,pentosanases, malanases, β-glucanases, arabinosidases, hyaluronidase,chondroitinase, laccase, and amylases, or mixtures thereof. A typicalcombination is a cocktail of conventional applicable enzymes likeprotease, lipase, cutinase and/or cellulase in conjunction with amylase.

Enzyme Stabilizers—Enzymes for use in compositions, for example,detergents can be stabilized by various techniques. The enzymes employedherein can be stabilized by the presence of water-soluble sources ofcalcium and/or magnesium ions in the finished compositions that providesuch ions to the enzymes.

Catalytic Metal Complexes—Applicants' compositions may include catalyticmetal complexes. One type of metal-containing bleach catalyst is acatalyst system comprising a transition metal cation of defined bleachcatalytic activity, such as copper, iron, titanium, ruthenium, tungsten,molybdenum, or manganese cations, an auxiliary metal cation havinglittle or no bleach catalytic activity, such as zinc or aluminumcations, and a sequestrate having defined stability constants for thecatalytic and auxiliary metal cations, particularlyethylenediaminetetraacetic acid, ethylenediaminetetra(methyl-enephos-phonic acid) and water-soluble salts thereof. Suchcatalysts are disclosed in U.S. Pat. No. 4,430,243.

If desired, the compositions herein can be catalyzed by means of amanganese compound. Such compounds and levels of use are well known inthe art and include, for example, the manganese-based catalystsdisclosed in U.S. Pat. No. 5,576,282.

Cobalt bleach catalysts useful herein are known, and are described, forexample, in U.S. Pat. Nos. 5,597,936 and 5,595,967. Such cobaltcatalysts are readily prepared by known procedures, such as taught forexample in U.S. Pat. Nos. 5,597,936, and 5,595,967.

Compositions herein may also suitably include a transition metal complexof a macropolycyclic rigid ligand—abbreviated as “MRL”. As a practicalmatter, and not by way of limitation, the compositions and cleaningprocesses herein can be adjusted to provide on the order of at least onepart per hundred million of the benefit agent MRL species in the aqueouswashing medium, and may provide from about 0.005 ppm to about 25 ppm,from about 0.05 ppm to about 10 ppm, or even from about 0.1 ppm to about5 ppm, of the MRL in the wash liquor.

Preferred transition-metals in the instant transition-metal bleachcatalyst include manganese, iron and chromium. Preferred MRL's hereinare a special type of ultra-rigid ligand that is cross-bridged such as5,12-diethyl-1,5,8,12-tetraazabicyclo[6.6.2]hexa-decane.

Suitable transition metal MRLs are readily prepared by known procedures,such as taught for example in WO 00/32601, and U.S. Pat. No. 6,225,464.

Processes of Making and Using Compositions

The compositions of the present invention can be formulated into anysuitable form and prepared by any process chosen by the formulator,non-limiting examples of which are described in U.S. Pat. No. 5,879,584;U.S. Pat. No. 5,691,297; U.S. Pat. No. 5,574,005; U.S. Pat. No.5,569,645; U.S. Pat. No. 5,565,422; U.S. Pat. No. 5,516,448; U.S. Pat.No. 5,489,392; U.S. Pat. No. 5,486,303 all of which are incorporatedherein by reference.

Method of Use

Compositions containing the encapsulated benefit agent disclosed hereincan be used to clean or treat a situs inter alia a surface or fabric.Typically at least a portion of the situs is contacted with anembodiment of Applicants' composition, in neat form or diluted in aliquor, for example, a wash liquor and then the situs may be optionallywashed and/or rinsed. In one aspect, a situs is optionally washed and/orrinsed, contacted with a one or more of the benefit agent deliverycompositions of the present invention or a consumer product comprisingone or more of the benefit agent delivery compositions of the presentinvention and then optionally washed and/or rinsed. For purposes of thepresent invention, washing includes but is not limited to, scrubbing,and mechanical agitation. The fabric may comprise most any fabriccapable of being laundered or treated in normal consumer use conditions.Liquors that may comprise the disclosed compositions may have a pH offrom about 3 to about 11.5. Such compositions are typically employed atconcentrations of from about 500 ppm to about 15,000 ppm in solution.When the wash solvent is water, the water temperature typically rangesfrom about 5° C. to about 90° C. and, when the situs comprises a fabric,the water to fabric ratio is typically from about 1:1 to about 30:1.

Test Methods

It is understood that the test methods that are disclosed in the TestMethods Section of the present application should be used to determinethe respective values of the parameters of Applicants' invention as suchinvention is described and claimed herein.

(1) ClogP

-   -   The “calculated logP” (ClogP) is determined by the fragment        approach of Hansch and

Leo (cf., A. Leo, in Comprehensive Medicinal Chemistry, Vol. 4, C.Hansch, P. G. Sammens, J. B. Taylor, and C. A. Ramsden, Eds. P. 295,Pergamon Press, 1990, incorporated herein by reference). ClogP valuesmay be calculated by using the “CLOGP” program available from DaylightChemical Information Systems Inc. of Irvine, Calif. U.S.A.

(2) Boiling Point

-   -   Boiling point is measured by ASTM method D2887-04a, “Standard        Test Method for Boiling Range Distribution of Petroleum        Fractions by Gas Chromatography,” ASTM International.

(3) Free Formaldehyde

-   -   Free formaldehyde is measured in accordance with NIOSH 5700 with        the following adaptations:    -   Adaptation of DNPH concentration: minimize polymer degradation        during derivatization reaction and create condition to monitor        fate of derivatization reagent during subsequent LC analysis        (check for potential reagent consumption by other sample        constituents such as perfume carbonyls).    -   Reduction of the acid concentration and use of hydrochloric acid        instead of perchloric acid: create milder conditions for        derivatization, avoiding excessive polymer/resin degradation.        (Derivatization kinetics at these conditions are checked to show        reaction plateau is reached at about 10 min>>do we need to        incorporate these reaction kinetics curves or not?).    -   Solvent extraction (Acetonitrile): ensures fast separation of        the solid material from samples and allowing for easy        filtration. The filtrate contains formaldehyde for analysis.        Standard calibration solutions are made up to match the solvent        composition to that of samples analyzed to ensure equal reaction        conditions for derivatization.

Test Protocol & Apparatus Apparatus

-   1) Waters HPLC instrumentation and Millennium system control and    data acquisition system.-   2) Continuous flow eluent vacuum degassing unit (Erma ERC-3612 or    equivalent. Alternatively use He sparging)-   3) Solvent delivery module (Waters 600E or equivalent multiple    channel solvent delivery system)-   4) Variable volume injector (Waters 717 plus, automatic injector or    equivalent)-   5) Analytical HPLC column/guard column (Symmetry C8, 3.9×1 50 mm,    WAT no 054235 with guard column WAT no 054250 or equivalent)-   6) UV detector (Waters 996 Photo Diode Array Detector or    equivalent) 7) Data station (Waters Millennium 2010, 2020 C/S, or an    equivalent system capable of storing and processing data).-   8) Disposable filter units (0.45 μm, PTFE or 0.45 μm 25 mm, for    sample filtration. Millipore Millex HV, cat. no. SLSR025NS)-   9) Disposable syringes (Polypropylene 2 mL, with Luer fitting. Must    match filtration unit female Luer.-   10) Disposable glass sample vials, 4 mL, with caps. (Waters 4 mL    clear glass vials with caps No. WAT025051, or equivalent)-   11) Disposable filter cups, 0.45 μm, for eluent filtration.    Millipore, cat no. SJHVM4710, or equivalent.-   12) Lab Shaker+Lab Therm (Applitek Scientific Instruments or    equivalent)-   13) Titration equipment consisting of:    -   a. Automatic titrator (Mettler DL70 or equivalent)    -   b. Platinum electrode (Mettler DM140-Sc or equivalent)    -   c. Titration vessel (100 mL, fitting DL70 or an equivalent        automatic titrator system)

Reagents And Solutions Reagents/Solvents

-   -   (1) HPLC grade water (Resistivity above 18 free from organic        material.    -   (2) Acetonitrile (HPLC Ultra Gradient Grade, J. T. Baker, no.        9017 or equivalent)    -   (3) Ion Pair Reagent: tetrabutylammonium hydrogen sulfate Pic        reagent A Low UV, Waters no. WAT084189 or equivalent    -   (4) 2,4-dinitrophenylhydrazine (C₆H₆N₄O₄) Aldrich no 19,930-3 or        equivalent    -   (5) Formaldehyde 37 wt. % in water, used as standard material.        Aldrich, no 25,254-9 or equivalent    -   (6) Ethanol absolute (J T Baker, no. 8006 or equivalent)    -   (7) Hydrochloric acid 36-38% (JT. Baker, no 6081 or equivalent)    -   (8) Iodine, volumetric standard, 0.1N solution in water Aldrich,        no 31,898-1 or equivalent    -   (9) Sodium hydroxide, 1N (Aldrich, no 31,951-1 or equivalent)    -   (10) Hydrochloric acid, 1N (Aldrich, no 31,894-9 or equivalent)    -   (11) Sodium thiosulphate, volumetric standard, 0.1N solution in        water Aldrich, no 31,954-6 or equivalent

Solutions

-   -   (1) Eluent A: water/ACN 90:10 with 5 mM Pic. Dissolve one bottle        of Pic A Low UV into 900 mL of HPLC grade water. Add, while        stirring vigorously, 100 mL of acetonitrile. Filter through a        0.45 μm disposable filter cup.    -   (2) Eluent B: water/ACN 30:70 with 5 mM Pic A. Dissolve one        bottle of Pic A Low UV into 300 mL of HPLC grade water. Add very        slowly, while stirring vigorously, 700 mL of acetonitrile.        Filter through a 0.45 μm disposable filter cup. It is very        important to mix well and add the acetonitrile very slowly to        prevent the precipitation of the Pic A as much as possible.        Preferably, prepare this eluent well in advance to allow        equilibration and avoid precipitation during use. Filter before        use.    -   (3) 2,4 Dinitrophenylhydrazine stock solution. Weigh, to the        nearest 0.01 g, 0.4 g of 2,4-DNPH in a 100 mL glass bottle. Add        20 ml of ethanol absolute and stir vigorously. While stirring,        add slowly 16 ml of concentrated hydrochloric acid, followed by        64 ml of ethanol absolute. The 2,4-DNPH stock solution can be        kept for about 2 months.    -   (4) 2,4 Dinitrophenylhydrazine working solution for samples.        Pipette 5 mL of the 2,4-dinitrophenylhydrazine stock solution        into a 100 mL glass volumetric flask. Fill to volume with de        ionized water and mix well. The 2,4-DNPH working solution has to        be re-made daily.    -   (5) 2,4 Dinitrophenylhydrazine working solution for standards.        Pipette 5 mL of the 2,4-dinitophenylhydrazine stock solution        into a 100 mL glass volumetric flask. Fill to volume with        acetonitrile mix well. The 2,4-DNPH working solution has to be        re-made daily.

Procedure

-   -   1) Formaldehyde standard stock solution: Weigh, to the nearest        0.0001 gram, 1.0 g of formaldehyde standard into a small sample        cup. Dissolve into a 1 L volumetric flask using deionized water.        Record the weight as Wst    -   2) Preparation of standard working solutions        -   a. Pipette 5 mL of the formaldehyde stock solution into a 50            mL volumetric flask. Bring to volume with de ionized water            and mix well.        -   b. Pipette 0, 0.5, 1.0, 3, and 5 mL of the diluted stock            solution into separate 50 mL volumetric flasks. Bring to            volume with de ionized water and mix well. Filter            approximately 5 mL of each standard working solution through            a 0.45 μm disposable filter unit into a glass vial.    -   3) Sample preparation: Weigh, to the nearest 0.0001 gram, about        1 gram of sample into a 50 mL volumetric flask. Bring to volume        with acetonitrile and mix well. Allow about five (5) minutes for        the insoluble material to settle. Filter approximately 5 mL of        the sample solution through a 0.45 μm disposable filter unit        into a glass vial. Record the exact weight as Wsa in grams.    -   4) Derivatization procedure        -   a. Pipette 1.00 mL of each standard solution, filtered            sample solution, and filtered extract into separate 4 mL            sample vials. The choice of the calibration range is            dependent on the expected free formaldehyde level in sample            solutions or extracts.        -   b. Standards: add 1.00 mL of 2,4-DNPH working solution for            standards to each vial. Stopper and mix.        -   c. Samples: add 1.00 mL of 2,4-DNPH working solution for            samples to each vial. Stopper and mix.        -   d. Let react for 10 minutes±20 seconds before injection.            Note: this timing is critical. Start the timer as soon as            the reagents are mixed and take into account the time it            takes to load and inject a sample.    -   5) Instrumental Operation: Set up the HPLC system according to        the manufacturer's instructions using the following conditions:        -   Isocratic: 20% A-80% B/0.8 ml/min        -   Detection: UV at 365 nm        -   Inj. volume: 20 μl        -   Runtime: 10 minutes

Calibration

-   -   1) Inject 20 μl of a derivatized standard solution at least once        to check for proper instrument functioning (Never use the area        counts of the first injection for calibration purposes. The        first injection after start up of the HPLC system is generally        not representative).    -   2) Inject 20 μl of each of the derivatized standard solutions.    -   3) Record the peak areas and, with the help of the examples in        appendix 9, assign the peak identity.

Analysis of the Samples

-   -   1) Inject 20 μl of each of the derivatized sample solutions or        extracts.    -   2) Record the peak area for the formaldehyde peak.    -   3) After analyses are finished, replace the eluent by de ionized        water and then a storage solvent, e.g. HPLC grade methanol,        before removing the column from the system.

Calculations

(1) Calculate the amount of formaldehyde in each of the standardsolutions (calibration range: 0-5 μg/mL)

${\underset{\_}{vol}\mspace{14mu} {\mu g}\mspace{14mu} {formaldehyde}\text{/}{mL}} = {\frac{{Wst} \times {Ast} \times 1000 \times {Dil}\mspace{14mu} {vol}}{100 \times 10 \times 50} = \frac{{Wst} \times {Ast} \times {Dil}}{50}}$

-   -   Where:        -   Wst=weight of standard in the stock solution in grams            (7.1.1)        -   Ast=Activity of the standard material (%) determined by            titration (7.1.5)        -   Dil vol=diluted standard stock amounts in mL used for            preparing standard solutions (0-10 mL)            (2) Construct a calibration curve (amounts versus peak            area). When using the Waters Millennium 2010 data processing            software, perform the ‘Fit Type’: Linear calibration setting            in ‘Component table’ of the Processing Method            (3) Starting from the formaldehyde peak area of a sample,            read the amount of formaldehyde in the sample solution or            extract in μg/mL from the calibration curve. Record this            value as μg_(sa) Note: this calculation assumes that            injection volumes of standards and samples are identical.

(4) Calculate the amount of formaldehyde in the samples as follows:

${{ppm}\mspace{14mu} {form}\; {aldehyde}} = \frac{\mu \; {gsa} \times 100}{Wsa}$

Where: μgsa=amount of free formaldehyde in the sample solution in μg/mL(7.3)

-   -   Wsa=weight of sample in grams (7.3.1)

EXAMPLES

While particular embodiments of the present invention have beenillustrated and described, it would be obvious to those skilled in theart that various other changes and modifications can be made withoutdeparting from the spirit and scope of the invention. It is thereforeintended to cover in the appended claims all such changes andmodifications that are within the scope of this invention.

Example 1

80 wt % Core/20 wt % Wall Melamine Formaldehyde (MF) Capsule 18 grams ofa blend of 50% butyl acrylate-acrylic acid copolymer emulsifier (ColloidC351, 25% solids, pka 4.5-4.7, Kemira) and 50% polyacrylic acid (35%solids, pKa 1.5-2.5, Aldrich) is dissolved and mixed in 200 gramsdeionized water. The pH of the solution is adjusted to pH of 3.5 withsodium hydroxide solution. 6.5 grams of partially methylated methylolmelamine resin (Cymel 385, 80% solids Cytec) is added to the emulsifiersolution. 200 grams of perfume oil is added to the previous mixtureunder mechanical agitation and the temperature is raised to 60° C. Aftermixing at higher speed until a stable emulsion is obtained, the secondsolution and 3.5 grams of sodium sulfate salt are poured into theemulsion. This second solution contains 10 grams of butylacrylate-acrylic acid copolymer emulsifier (Colloid C351, 25% solids,pka 4.5-4.7, Kemira), 120 grams of distilled water, sodium hydroxidesolution to adjust pH to 4.6, 30 grams of partially methylated methylolmelamine resin (Cymel 385, 80% Cytec). This mixture is heated to 75° C.and maintained 6 hours with continuous stirring to complete theencapsulation process. An average capsule size of 20 um is obtained asanalyzed by a Model 780 Accusizer. The measured free formaldehydeconcentration in the perfume microcapsule slurry is 5000 ppm.

Example 2

84 wt % Core/16 wt % Wall Melamine Formaldehyde (MF) Capsule 25 grams ofbutyl acrylate-acrylic acid copolymer emulsifier (Colloid C351, 25%solids, pka 4.5-4.7, (Kemira Chemicals, Inc. Kennesaw, Ga. U.S.A.) isdissolved and mixed in 200 grams deionized water. The pH of the solutionis adjusted to pH of 4.0 with sodium hydroxide solution. 8 grams ofpartially methylated methylol melamine resin (Cymel 385, 80% solids,(Cytec Industries West Paterson, N.J., U.S.A.)) is added to theemulsifier solution. 200 grams of perfume oil is added to the previousmixture under mechanical agitation and the temperature is raised to 50°C. After mixing at higher speed until a stable emulsion is obtained, thesecond solution and 4 grams of sodium sulfate salt are added to theemulsion. This second solution contains 10 grams of butylacrylate-acrylic acid copolymer emulsifier (Colloid C351, 25% solids,pka 4.5-4.7, Kemira), 120 grams of distilled water, sodium hydroxidesolution to adjust pH to 4.8, 25 grams of partially methylated methylolmelamine resin (Cymel 385, 80% solids, Cytec). This mixture is heated to70° C. and maintained overnight with continuous stirring to complete theencapsulation process. An average capsule size of 20 um is obtained asanalyzed by a Model 780 Accusizer. The measured free formaldehydeconcentration in the perfume microcapsule slurry is 3500 ppm.

Example 3 Spray Drying

The perfume microcapsule slurry of Example 1 is pumped at a rate of 1kg/hr into a co-current spray dryer (Niro Production Minor, 1.2 meterdiameter) and atomized using a centrifugal wheel (100 mm diameter)rotating at 18,000 RPM. Dryer operating conditions are: air flow of 80kg/hr, an inlet air temperature of 200 degrees Centigrade, an outlettemperature of 100 degrees Centigrade, dryer operating at a pressure of−150 millimeters of water vacuum. The dried powder is collected at thebottom of a cyclone. The collected particles have an approximateparticle diameter of 20 microns. The measured free formaldehyde is 5000milligrams per liter. The equipment used the spray drying process may beobtained from the following suppliers: IKA Werke GmbH & Co. KG, Jankeand Kunkel—Str. 10, D79219 Staufen, Germany; Niro A/S Gladsaxevej 305,P.O. Box 45, 2860 Soeborg, Denmark and Watson-Marlow Bredel PumpsLimited, Falmouth, Cornwall, TR11 4RU, England.

Example 4 Solvent Exchange

150 grams of propylene glycol is added to 100 grams of the perfumemicrocapsules of Example 1. The mixture is prepared at 25 C, and placedin a rotary flash evaporator (Buchi Rotavapor R-114). A water bath(Baxter Scientific Products Durabath) is used to heat and maintain themixture at 65 C for 6 hours, with an initial vacuum of 15 inches ofmercury that is raised to 28.2 inches of mercury over the duration ofthe evaporation (Welch 1400 DuoSeal vacuum pump). The rate of vacuumincrease is governed by the amount of water in the mixture andminimizing the risk of “popping” over the mixture. The final watercontent is measured to be 1.1 wt %, solids content of 21%, and the freeformaldehyde in the slurry is 2990 milligrams per liter.

200 grams of glycerol is added to 100 grams of the perfume microcapsulesof Example 1. The mixture is prepared at 25 C, and placed in a rotaryflash evaporator (Buchi Rotavapor R-114). A water bath (BaxterScientific Products Durabath) is used to heat and maintain the mixtureat 65 C for 8 hours, with an initial vacuum of 15 inches of mercury thatis raised to 28.2 inches of mercury over the duration of the evaporation(Welch 1400 DuoSeal vacuum pump). The rate of vacuum increase isgoverned by the amount of water in the mixture and minimizing the riskof “popping” over the mixture. The final water content is 2 wt %, solidscontent is 17 wt %, and the free formaldehyde in the slurry is 2550milligrams per liter.

Example 5 Batch Filtration

Example 5B is prepared by mixing 50 grams of the perfume microcapsuleslurry of Example 1 (pH 5.0) with 60 grams of deionized water. Themixture is heated to 65 degrees Centigrade. The mixture is then pouredonto a batch filter assembly. The batch filter assembly comprises aBuchner funnel with a 250 micron sieve, onto which is laid a membrane(WPP807—wound polypropylene, 15 micron pore size; or 2.0 SM—spunboundmeltblown nonwoven, 17 micron pore size), filtration area of 0.011square feet. The entire assembly can be pressurized up to 40 psigpressure. The permeate passes through the membrane, then through thelarge pore sieve, and is collected. After adding the perfumemicrocapsule mixture onto the membrane, the entire assembly ispressurized to 40 psig. The rate of permeate collection is monitored.The assembly is depressurized after 3 minutes, and the dewatered perfumemicrocapsule cake is removed.

Mass of Mass of Free Total Example Example 1 Water CH₂O in Free CH₂OCH₂O in ID Membrane Slurry (g) Added (g) Cake in Permeate Slurry 5AWPP807 50 0 2593 7118 4403 5B WPP807 50 30 1407 4093 4264 5E 2.0SM 50 01983 7006 3992 5F 2.0SM 50 30 1407 3807 4153

Example 6 Batch Filtration

The 2.0SM membrane of Example 5 shows the best results for minimizingfree formaldehyde in the filtered cake. This membrane is utilized todetermine the effect of pre-dilution and pH adjustment (with 50 wt %citric acid) of the perfume microcapsules of Example 1.

Mass of deionized water added to 50 grams Example of perfumemicrocapsules Free Formaldehyde in a PMC ID of Example 1 (pH 5.0) Cake6A 0 3259 6B 30 2416 6C 60 1917 6D 90 1906 6E 120 1779 6F 150 1527

Example Free Formaldehyde ID Description (milligrams per liter) 6GExample 1, pH 2.5 Cake 1047 6H Example 1, pH 2.0 Cake 1061 6I Example 1,pH 1.5 Cake 1236

The expected free formaldehyde in the samples above is 1000 milligramsper liter (based on the quantity of formaldehyde in the sampleinitially, and removal of water during the filtration process). Thefiltered cakes 6G, 6H, and 6I are reconstituted in an aqueous slurry toyield a phase stable suspension in the following way: to 20.8 grams ofthe filtered cake is added 10.6 grams of DI water, then 6.0 grams of 1wt % aqueous solution of Optixan Xanthan Gum (ADM Corporation), and 2.50grams of 32 wt % magnesium chloride solution. The aqueous suspensionsare aged 1 week at 25° C., prior to measuring the free formaldehyde.

Expected Free Free Formaldehyde Formaldehyde Example (milligrams(milligrams per ID Description per liter) liter) 6J Cake 6G,reconstituted 1329 480 6K Cake 6H, reconstituted 1524 480 6L Cake 6I,reconstituted 1857 480

There is a “reservoir” of formaldehyde that generates free formaldehydein the bulk solution. This “reservoir” cannot be eliminated bydilution+filtering, nor reducing the pH of the slurry prior tofiltration.

Example 7 Continuous Filtration

Continuous diafiltration of the PMC slurry is completed through twodifferent sized membranes—0.14 micron (Zirconium Dioxide+TitaniumDioxide, from TAMI Industries of France), and 300 kilo Dalton (ZirconiumDioxide, from TAMI Industries of France). 3 parts water is added to 1part of perfume microcapsules of Example 1 (but with free formaldehydein the bulk adjusted to 1200 ppm using acetoacetamide as a scavenger).This slurry is then used to determine the ideal flowrate through thex-membrane filter by running the continuous filtration operation at 4different flow rates, and measuring the permeate collection rate, andthe pressure drop across the membrane. The optimum transmembranepressure drop and flowrate that maximize permeate collection rate isfound to be 300 Liters per hour and 4 bar for the 300 kDa membrane, and230 Liters per hour and 5 bar for the 0.14 micron membrane. Then, theslurry is filtered across each membrane 5 times (in order to remove allof the water that had been added to the slurry). This constitutes 1pass. The material is then again diluted with 3 parts water for every 1part diafiltered slurry. The slurry is then filtered across the membraneto remove the added water. This constitutes 2 passes. A total of 5passes through the diafilter membrane are completed with each of themembranes.

Free Example Formaldehyde ID Description (ppm) 7A 3:1 water:PMC slurrydilution, no 316.5 diafiltration 7B 1 pass diafiltration, 0.14 micronmembrane 300.4 7C 2 pass diafiltration, 0.14 micron membrane 332.3 7D 3pass diafiltration, 0.14 micron membrane 250.1 7E 4 pass diafiltration,0.14 micron membrane 196.5 7F 5 pass diafiltration, 0.14 micron membrane106.7 7G 1 pass diafiltration, 300 kDa membrane N/A 7H 2 passdiafiltration, 300 kDa membrane 355.3 7I 3 pass diafiltration, 300 kDamembrane 243.6 7J 4 pass diafiltration, 300 kDa membrane 183.9 7K 5 passdiafiltration, 300 kDa membrane 148.2 Note that there is not asignificant reduction in free formaldehyde (there is a “reservoir” offormaldehyde).

Example 8 Batch Centrifuge

14 milliliters of the aqueous suspension of perfume microcapsules ofExample 1 are placed in a 20 milliliter centrifuge tube. 6 identicaltubes are prepared and placed in a batch centrifuge (IEC Centra CL2).After 20 minutes at 3800 RPM, the centrifuge tubes are removed, andthree layers are observed: perfume microcapsule cake layer on top,followed by an aqueous layer, followed by a high density solidparticulate layer. The top microcapsule layer is isolated from theremaining material, and submitted for free formaldehyde analysis. Themicrocapsule cake is also reconstituted to make a phase stablesuspension (To 20.8 grams of the top perfume microcapsule layer is added10.6 grams of DI water, then 6.0 grams of 1 wt % aqueous solution ofOptixan Xanthan Gum from ADM Corporation, and 2.50 grams of 32 wt %magnesium chloride solution from Chemical Ventures). Free formaldehydein PMC layer (top layer) is measured to be 2244 milligrams per liter.Free Formaldehyde in the reconstituted microcapsules (2 wk/25 C aged) ismeasured to be 1083 milligrams per liter. The free formaldehyde showsthe expected trend, a decrease in level that is proportional to theamount of dilution water that is added. i.e. the “reservoir” offormaldehyde has been removed by this physical separation technique.

Example 9 Batch Centrifuge

The perfume microcapsules slurry of Example 2 is pH adjusted with 50 wt% citric acid. 14 milliliters of the aqueous suspension of perfumemicrocapsules of Example 2 are placed in a 20 milliliter centrifugetube. 6 identical such tubes are prepared and placed in a batchcentrifuge (IEC Centra CL2). After 20 minutes at 3800 RPM, thecentrifuge tubes are removed, and three layers are observed: perfumemicrocapsule cake layer on top, followed by an aqueous layer, followedby a high density solid particulate layer. The top microcapsule layer isisolated from the remaining material. To 20.8 grams of the top perfumemicrocapsule layer is added 10.6 grams of DI water, then 6.0 grams of 1wt % aqueous solution of Optixan Xanthan Gum from ADM Corporation, and2.50 grams of 32 wt % magnesium chloride solution from ChemicalVentures. The top microcapsule layer, and the reconstituted perfumemicrocapsule slurry are analyzed for free formaldehyde content (Example9A, 9B).

Example Free CH2O Free CH2O ID Description (cake) (reconstituted) 8A, 8BExample 2 (pH 5.3) Batch 2244 1083 Centrifuge (CONTROL) 9A, 9B Example2, pH 2.5, Batch 2151 1141 Centrifuge

Example 10 Batch Centrifuge

14 milliliters of the aqueous suspension of perfume microcapsules ofExample 2 are placed in a 20 milliliter centrifuge tube. 6 identicalsuch tubes are prepared and placed in a batch centrifuge (IEC CentraCL2). After 20 minutes at 3800 RPM, the centrifuge tubes are removed,and three layers are observed: perfume microcapsule cake layer on top,followed by an aqueous layer, followed by a high density solidparticulate layer. The top microcapsule layer is isolated from theremaining material. 4 grams of the top microcapsule layer is mixed with8 grams of deionized water. 4 identical such tubes are prepared andbatch centrifuged. The top microcapsule layer from the centrifuged tubesis removed and free formaldehyde is analyzed (Example 10A, 2 passes).

4 grams of the top microcapsule layer of Example 8E is mixed with 8grams of deionized water. 2 identical such tubes are prepared and batchcentrifuged (IEC Centra CL2, 20 minutes at 3800 RPM, 25 C). The topmicrocapsule layer from the centrifuge tubes is isolated and analyzedfor free formaldehyde (Example 10B, 3 passes). The analysis shows thatone can permanently remove free formaldehyde from the perfumemicrocapsules by increasing the number of centrifuge cycles.

Example Free CH₂O Free CH₂O ID Description (cake) (reconstituted) 8A, 8BExample 2 (pH 5.3) - 1 pass 2244 1083 Batch Centrifuge 10A Example 2 (pH5.3) - 2 passes 581 N/A Batch Centrifuge 10B Example 2 (pH 5.3) - 3passes 326 N/A Batch Centrifuge

The perfume microcapsule cakes 8A, 10A, and 10B are reconstituted inwater (To 20.8 grams of the top perfume microcapsule layer is added 10.6grams of DI water, then 6.0 grams of 1 wt % aqueous solution of OptixanXanthan Gum from ADM Corporation, and 2.50 grams of 32 wt % magnesiumchloride solution from Chemical Ventures), and aged for 96 hours at 35degrees Centigrade.

Free CH₂O (reconstituted, Example Free CH₂O aged ID Description (cake)96 hr/35° C.)  8A, 10C Example 2 (pH 5.3) - 1 pass 2244 1466 BatchCentrifuge 10A, 10D Example 2 (pH 5.3) - 2 passes 581 594 BatchCentrifuge 10B, 10E Example 2 (pH 5.3) - 3 passes 326 411 BatchCentrifuge

There is a rise in free formaldehyde from 1083 ppm to 1466 ppm for theonce centrifuged slurry. Multiple centrifuge cycles are efficient inreducing the rise of free formaldehyde upon ageing.

The pH adjustment of perfume microcapsules of Example 2 yields asignificant rise in releasable formaldehyde (3116 ppm to 6100 ppm). Thecentrifuged perfume microcapsules yield a much lesser rise in releasableformaldehyde, indicating that a large reservoir of free formaldehyde hasbeen removed during the centrifugation process.

Free CH₂O Reconstituted Slurry pH Free CH₂O adjusted 2.5 ExampleReconstituted 1 wk/25° C. ID Description Slurry pH 4.3 ageing  8B, 10FExample 2 (pH 5.3) - 1 1083 1216 pass Batch Centrifuge 10G, 10H Example2 (pH 5.3) - no 3116 6100 centrifuge

Example 11 Reactive Adsorption

Approximately 1.0 grams of the perfume microcapsules of Example 1 areplaced into a glass jar. Approximately 1.0 grams of deionized water isadded to the jar. Polymeric resin is then added to the diluted perfumemicrocapsule slurry. The sample is speed mixed at 3000 RPM for 2 minutesand allowed to sit overnight at 25 degrees Centigrade. The sample isspeed mixed the next morning at 3000 RPM for 2 minutes. The slurry isfiltered to remove the polymeric resin, and free formaldehyde ismeasured. A description of the experiments is summarized in the tablebelow. The free formaldehyde of the perfume microcapsule slurry prior toany addition of polymeric resins is measured to be 4800 ppm.

Measured Mass of Mass of Free Resin/Scavenger slurry (g) water (g)Formaldehyde ScavengePore ®-aminomethylated 1.1175 1.0000 63.0polystyrene Poly (4-vinylpyridine) 1.0218 1.0000 5060.8Diethylenetriamine, polymer-bound 1.0614 1.0000 3477.1p-Toluenesulfonylhydrazide, polymer-bound 1.0608 1.0000 183.5 10%PVOH/PVAm M12 solution 1.0452 0.0000 3611.4ScavengePore ®-aminomethylated 2.0137 2.0175 76.9 polystyreneScavengePore ®-aminomethylated 2.0821 1.0936 67.1 polystyrenep-Toluenesulfonylhydrazide, polymer-bound 2.0017 2.0399 59.8p-Toluenesulfonylhydrazide, polymer-bound 2.0099 0.0000 142.1ArgoPore ®-NH₂ HL 2.0059 1.0023 3.6 JandaJel-NH₂ 2.0319 1.0020 505.0StratoSpheres PL-AMS 2.0042 1.0021 831.8 StratoSpheres PL-AMS 2.12621.0022 654.4 Aminomethyl polymer resin 2.0041 1.0021 551.0ArgoPore ®-NH2 HL 2.0059 1.0023 146.9

Example 12 Finished Product Compositions

Non-limiting examples of product formulations containing purifiedperfume microcapsules of the aforementioned examples are summarized inthe following table.

EXAMPLES (% wt) A B C D E F G H I J FSA^(a) 14 16.47 14 12 12 16.47 — —5 5 FSA^(b) — 3.00 — — — FSA^(c) — — 6.5 — — Ethanol 2.18 2.57 2.18 1.951.95 2.57 — — 0.81 0.81 Isopropyl — — — — — — 0.33  1.22 — — AlcoholStarch^(d) 1.25 1.47 2.00 1.25 — 2.30 0.5  0.70 0.71 0.42 Microcapsule(% 0.6 0.75 0.6 0.75 0.37 0.60 0.37 0.6 0.37 0.37 active)* PhaseStabilizing 0.21 0.25 0.21 0.21 0.14 — —  0.14 — — Polymer^(f) SudsSuppressor^(g) — — — — — — — 0.1 — — Calcium 0.15 0.176 0.15 0.15 0.300.176 — 0.1-0.15 — — Chloride DTPA^(h) 0.017 0.017 0.017 0.017 0.0070.007 0.20 — 0.002 0.002 Preservative 5 5 5 5 5 5 —  250^(j)    5 5(ppm)^(i,j) Antifoam^(k) 0.015 0.018 0.015 0.015 0.015 0.015 — — 0.0150.015 Dye 40 40 40 40 40 40 11 30-300 30 30 (ppm) Ammonium 0.100 0.1180.100 0.100 0.115 0.115 — — — — Chloride HCl 0.012 0.014 0.012 0.0120.028 0.028 0.016  0.025 0.011 0.011 Structurant^(l) 0.01 0.01 0.01 0.010.01 0.01 0.01  0.01 0.01 0.01 Neat 0.8 0.7 0.9 0.5 1.2 0.5 1.1 0.6 1.00.9 Unencapsulated Perfume Deionized Water Balance Balance BalanceBalance Balance Balance Balance Balance Balance Balance^(a)N,N-di(tallowoyloxyethyl)-N,N-dimethylammonium chloride. ^(b)Methylbis(tallow amidoethyl)2-hydroxyethyl ammonium methyl sulfate.^(c)Reaction product of Fatty acid with Methyldiethanolamine in a molarratio 1.5:1, quaternized with Methylchloride, resulting in a 1:1 molarmixture of N,N-bis(stearoyl-oxy-ethyl) N,N-dimethyl ammonium chlorideand N-(stearoyl-oxy-ethyl) N,-hydroxyethyl N,N dimethyl ammoniumchloride. ^(d)Cationic high amylose maize starch available from NationalStarch under the trade name CATO ®. ^(f)Copolymer of ethylene oxide andterephthalate having the formula described in U.S. Pat. No. 5,574,179 atcol.15, lines 1-5, wherein each X is methyl, each n is 40, u is 4, eachR1 is essentially 1,4-phenylene moieties, each R2 is essentiallyethylene, 1,2-propylene moieties, or mixtures thereof. ^(g)SE39 fromWacker ^(h)Diethylenetriaminepentaacetic acid. ^(i)KATHON ® CG availablefrom Rohm and Haas Co. “PPM” is “parts per million.” ^(j)Gluteraldehyde^(k)Silicone antifoam agent available from Dow Corning Corp. under thetrade name DC2310. ^(l)Hydrophobically-modified ethoxylated urethaneavailable from Rohm and Haas under the tradename Aculyn ™ 44. *Suitablecombinations of the microcapsules provided in Examples 1 through 7.(Percent active relates to the core content of the microcapsule.)

The formaldehyde levels of the compositions of Example 12 are measuredin accordance with Test Method 3 of the present specification are foundto have formaldehyde levels of less than 50 ppm.

Example 13 Microcapsules in Dry Laundry Formulations

Non-limiting examples of product formulations containing purifiedperfume microcapsules of the aforementioned examples are summarized inthe following table.

% w/w granular laundry detergent composition Component A B C D E F GBrightener 0.1 0.1 0.1 0.2 0.1 0.2 0.1 Soap 0.6 0.6 0.6 0.6 0.6 0.6 0.6Ethylenediamine disuccinic acid 0.1 0.1 0.1 0.1 0.1 0.1 0.1Acrylate/maleate copolymer 1.5 1.5 1.5 1.5 1.5 1.5 1.5 Hydroxyethanedi(methylene 0.4 0.4 0.4 0.4 0.4 0.4 0.4 phosphonic acid) Mono-C₁₂₋₁₄alkyl, di-methyl, 0.5 0.5 0.5 0.5 0.5 0.5 0.5 mono-hydroyethylquaternary ammonium chloride Linear alkyl benzene 0.1 0.1 0.2 0.1 0.10.2 0.1 Linear alkyl benzene sulphonate 10.3 10.1 19.9 14.7 10.3 17 10.5Magnesium sulphate 0.4 0.4 0.4 0.4 0.4 0.4 0.4 Sodium carbonate 19.519.2 10.1 18.5 29.9 10.1 16.8 Sodium sulphate 29.6 29.8 38.8 15.1 24.419.7 19.1 Sodium Chloride 0.1 0.1 0.1 0.1 0.1 0.1 0.1 Zeolite 9.6 9.48.1 18 10 13.2 17.3 Photobleach particle 0.1 0.1 0.2 0.1 0.2 0.1 0.2Blue and red carbonate speckles 1.8 1.8 1.8 1.8 1.8 1.8 1.8 EthoxylatedAlcohol AE7 1 1 1 1 1 1 1 Tetraacetyl ethylene diamine 0.9 0.9 0.9 0.90.9 0.9 0.9 agglomerate (92 wt % active) Citric acid 1.4 1.4 1.4 1.4 1.41.4 1.4 PDMS/clay agglomerates (9.5% 10.5 10.3 5 15 5.1 7.3 10.2 wt %active PDMS) Polyethylene oxide 0.2 0.2 0.2 0.2 0.2 0.2 0.2 Enzymes e.g.Protease (84 mg/g 0.2 0.3 0.2 0.1 0.2 0.1 0.2 active), Amylase (22 mg/gactive) Suds suppressor agglomerate 0.2 0.2 0.2 0.2 0.2 0.2 0.2 (12.4 wt% active) Sodium percarbonate (having 7.2 7.1 4.9 5.4 6.9 19.3 13.1 from12% to 15% active AvOx) Perfume oil 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Solidperfume particles 0.4 0 0.4 0.4 0.4 0.4 0.6 Perfume microcapsules* 1.32.4 1 1.3 1.3 1.3 0.7 Water 1.4 1.4 1.4 1.4 1.4 1.4 1.4 Misc 0.1 0.1 0.10.1 0.1 0.1 0.1 Total Parts 100 100 100 100 100 100 100 *Microcapsuleadded as 35% active slurry (aqueous solution). Core/wall ratio can rangefrom 80/20 up to 90/10 and average particle diameter can range from 5 μmto 50 μm, and can be purified via any of the aforementioned examples.

The formaldehyde levels of the compositions of Example 13 are measuredin accordance with Test Method 3 of the present specification are foundto have formaldehyde levels of less than 10 ppm.

Example 14 Liquid Laundry Formulations (HDLs)

Non-limiting examples of product formulations containing purifiedperfume microcapsules of the aforementioned examples are summarized inthe following table.

Ingredient HDL 1 HDL 2 HDL3 HDL4 HDL 5 HDL 6 Alkyl Ether Sulphate 0.000.50 12.0 12.0 6.0 7.0 Dodecyl Benzene 8.0 8.0 1.0 1.0 2.0 3.0 SulphonicAcid Ethoxylated Alcohol 8.0 6.0 5.0 7.0 5.0 3.0 Citric Acid 5.0 3.0 3.05.0 2.0 3.0 Fatty Acid 3.0 5.0 5.0 3.0 6.0 5.0 Ethoxysulfated 1.9 1.21.5 2.0 1.0 1.0 hexamethylene diamine quaternized Diethylene triaminepenta 0.3 0.2 0.2 0.3 0.1 0.2 methylene phosphonic acid Enzymes 1.200.80 0 1.2 0 0.8 Brightener (disulphonated 0.14 0.09 0 0.14 0.01 0.09diamino stilbene based FWA) Cationic hydroxyethyl 0 0 0.10 0 0.200 0.30cellulose Poly(acrylamide-co- 0 0 0 0.50 0.10 0 diallyldimethylammoniumchloride) Hydrogenated Castor Oil 0.50 0.44 0.2 0.2 0.3 0.3 StructurantBoric acid 2.4 1.5 1.0 2.4 1.0 1.5 Ethanol 0.50 1.0 2.0 2.0 1.0 1.0 1,2propanediol 2.0 3.0 1.0 1.0 0.01 0.01 Glutaraldehyde 0 0 19 ppm 0 13 ppm0 Diethyleneglycol (DEG) 1.6 0 0 0 0 0 2,3-Methyl-1,3- 1.0 1.0 0 0 0 0propanediol (M pdiol) Mono Ethanol Amine 1.0 0.5 0 0 0 0 NaOH SufficientTo pH 8 pH 8 pH 8 pH 8 pH 8 pH 8 Provide Formulation pH of: SodiumCumene 2.00 0 0 0 0 0 Sulphonate (NaCS) Silicone (PDMS) emulsion 0.0030.003 0.003 0.003 0.003 0.003 Perfume 0.7 0.5 0.8 0.8 0.6 0.6Polyethyleneimine 0.01 0.10 0.00 0.10 0.20 0.05 Perfume Microcapsules*1.00 5.00 1.00 2.00 0.10 0.80 Water Balance Balance Balance BalanceBalance Balance to to to to to to 100% 100% 100% 100% 100% 100%Microcapsule added as 35% active slurry (aqueous solution). Core/wallratio can range from 80/20 up to 90/10 and average particle diameter canrange from 5 μm to 50 μm, and can be purified via any of theaforementioned examples.

The formaldehyde levels of the compositions of Example 14 are measuredin accordance with Test Method 3 of the present specification are foundto have formaldehyde levels of less than 10 ppm.

Example 15

Non-limiting examples of product formulations containing purifiedperfume microcapsules of the aforementioned examples are summarized inthe following table.

Examples of liquid detergents A B C D C14-C15 alkyl poly ethoxylate (8)6.25 4.00 6.25 6.25 C12-C14 alkyl poly ethoxylate (7) 0.40 0.30 0.400.40 C12-C14 alkyl poly ethoxylate (3) sulfate Na 10.60 6.78 10.60 10.60salt Linear Alkylbenzene sulfonate acid 0.19 1.16 0.79 0.79 Citric Acid3.75 2.40 3.75 3.75 C12-C18 Fatty Acid 4.00 2.56 7.02 7.02 Enzymes 0.600.4 0.60 0.60 Boric Acid 2.4 1.5 1.25 1.25 Trans-sulphated ethoxylatedhexamethylene 1.11 0.71 1.11 1.11 diamine quat Diethylene triamine pentamethylene 0.17 0.11 0.17 0.17 phosphonic acid Fluorescent brightener0.09 0.06 0.14 0.14 Hydrogenated Castor Oil 0.05 0.300 0.20 0.20 Ethanol2.50 1.00 2.50 2.50 1,2 propanediol 1.14 0.7 1.14 1.14 Sodium hydroxide3.8 2.6 4.60 4.60 Mono Ethanol Amine 0.8 0.5 Na Cumene SulphonateSilicone emulsion 0.0030 0.0030 0.0030 0.0030 Dye 0.002 0.002 0.0020.002 Opacifier (Styrene Acrylate based) Bentonite Softening ClayAcrylamide/MAPTAC (ex Nalco Chemicals of 0.40 0.40 Naperville, IL)Mirapol 550 (ex Rhodia Chemie, France) Polyquaternium 10 - Cationichydroxyl ethyl cellulose PP-5495 (silicone ex Dow Corning Corporation,Midland, MI) DC 1664 (silicone ex Dow Corning Corporation, Midland, MI)Pearlescent agent* 0.2 Perfume micro capsules** (expressed as 0.8 0.51.0 0.7 perfume oil) Perfume 0.7 0.55 1.00 1.00 Poly Ethylene Imine MW25000 Water Up to Up to Up to Up to 100 100 100 100 *Mica-TiO₂ (PrestigeSilk Silver Star ex Eckart) or BiOCl (Biron Silver CO-Merck) orpre-crystallized EGDS (Tegopearl N 100 ex Degussa, expressed as pureEGDS) **Microcapsule added as 35% active slurry (aqueous solution).Core/wall ratio can range from 80/20 up to 90/10 and average particlediameter can range from 5 μm to 50 μm, and can be purified via any ofthe aforementioned examples.

Examples of liquid detergents E F G H C14-C15 alkyl poly ethoxylate (8)6.25 4.00 6.25 6.25 C12-C14 alkyl poly ethoxylate (7) 0.40 0.30 0.40C12-C14 alkyl poly ethoxylate (3) sulfate Na 10.60 6.78 10.60 10.60 saltLinear Alkylbenzene sulfonate acid 0.79 1.19 0.79 0.79 Citric Acid 3.752.40 3.75 3.75 C12-C18 Fatty Acid 7.02 4.48 7.02 7.02 Enzymes 0.60 1.00.60 Boric Acid 1.25 1.25 1.25 1.25 Trans-sulphated ethoxylatedhexamethylene 1.11 0.71 1.11 1.11 diamine quat Diethylene triamine pentamethylene 0.17 0.11 0.17 0.17 phosphonic acid Fluorescent brightener0.14 0.06 0.14 Hydrogenated Castor Oil 0.20 0.300 0.20 0.20 Ethanol 2.501.00 2.50 2.50 1,2 propanediol 1.14 0.09 1.14 1.14 Sodium hydroxide 4.603.01 4.60 4.60 Mono Ethanol Amine Na Cumene Sulphonate Silicone emulsion0.0030 0.0030 0.0030 0.0030 Dye 0.002 0.00084 0.00084 0.00084 Opacifier(Styrene Acrylate based) 0.1 Bentonite Softening Clay Acrylamide/MAPTAC(ex Nalco Chemicals of 0.40 Naperville, IL) Mirapol 550 (ex RhodiaChemie, France) 0.40 0.25 Polyquaternium 10 - Cationic hydroxyl ethyl0.30 cellulose PP-5495 (silicone ex Dow Corning 3.0 Corporation,Midland, MI) DC 1664 (silicone ex Dow Corning 3.0 3.0 Corporation,Midland, MI) Pearlescent agent* 0.2 Perfume micro capsules** (expressedas 0.9 0.3 0.5 1.2 perfume oil) Perfume 1.00 0.65 1.00 1.00 PolyEthylene Imine MW 25000 Water Up to Up to Up to Up to 100 100 100 100*Mica-TiO₂ (Prestige Silk Silver Star ex Eckart) or BiOCl (Biron SilverCO-Merck) or pre-crystallized EGDS (Tegopearl N 100 ex Degussa,expressed as pure EGDS) **Microcapsule added as 35% active slurry(aqueous solution). Core/wall ratio can range from 80/20 up to 90/10 andaverage particle diameter can range from 5 μm to 50 μm, and can bepurified via any of the aforementioned examples.

Examples of liquid detergents I J K C14-C15 alkyl poly ethoxylate (8)4.00 6.1 C12-C14 alkyl poly ethoxylate (7) 2.00 C12-C14 alkyl polyethoxylate (3) 6.78 sulfate Na salt Linear Alkylbenzene sulfonate acid1.19 7.8 15.0 Citric Acid 2.40 2.6 2.50 C12-C18 Fatty Acid 4.48 2.6 11.4Enzymes .55 .07 Boric Acid 1.25 1.50 1.3 Trans-sulphated ethoxylated0.71 1.20 hexamethylene diamine quat Diethylene triamine penta methylene0.11 0.20 0.7 phosphonic acid Fluorescent brightener 0.09 0.14Hydrogenated Castor Oil 0.300 0.45 0.09 Ethanol 1.00 1.40 0.7 1,2propanediol 0.09 3.30 6.7 Sodium hydroxide 3.01 3.00 5.5 Mono EthanolAmine 0.50 Na Cumene Sulphonate 1.6 Silicone emulsion 0.0030 0.0030 0.30Dye 0.00084 0.02 0.004 Opacifier (Styrene Acrylate based) BentoniteSoftening Clay 3.40 Acrylamide/MAPTAC (ex Nalco Chemicals of Naperville,IL) Mirapol 550 (ex Rhodia Chemie, France) Polyquaternium 10 - Cationic0.18 hydroxyl ethyl cellulose PP-5495 (silicone ex Dow CorningCorporation, Midland, MI) DC 1664 (silicone ex Dow Corning 3.0Corporation, Midland, MI) Pearlescent agent* 0.2 Perfume micro capsules(expressed 0.2 0.45 0.75 as perfume oil) Perfume 0.65 0.5 1.0 PolyEthylene Imine MW 25000 0.08 Water Up to Up to Up to 100 100 100Examples of liquid detergents L M** N C14-C15 alkyl poly ethoxylate (8)3.7 20.7 C12-C14 alkyl poly ethoxylate (7) 16.7 C12-C14 alkyl polyethoxylate (3) 17.8 5.5 sulfate Na salt Linear Alkylbenzene sulfonateacid 12.5 22.9 13.5 Citric Acid 3.9 1.7 C12-C18 Fatty Acid 11.1 18 5.1Enzymes 3 1.2 3 Boric Acid 0.5 0.5 Trans-sulphated ethoxylated 3.25 1.2hexamethylene diamine quat PEI 600 EO20 1.25 1.2 Diethylene triaminepenta methylene 1.6 0.85 phosphonic acid or HEDP Fluorescent brightener0.2 0.3 0.14 Hydrogenated Castor Oil 0.2 1,2 propanediol 4.3 20.3 11.7Sodium hydroxide 1.0 3.9 Mono Ethanol Amine 9.8 6.8 3.1 Dye PresentPresent Present PDMS 2.15 Potassium sulphite 0.2 Perfume micro capsules*(expressed 1.6 1.5 1.4 as perfume oil) Perfume 1.2 1.6 1.0 Form. PhenylBoronic Acid Present Water Up to Up to Up to 100 100 100 *Microcapsuleadded as 35% active slurry (aqueous solution). Core/wall ratio can rangefrom 80/20 up to 90/10 and average particle diameter can range from 5 μmto 50 μm, and can be purified via any of the aforementioned examples.**Low water liquid detergent in Polyvinylalcohol unidose/sachet

Example 16

A 25.36% perfume microcapsule slurry was pumped into a hermetic discstack centrifuge (Alfa Laval model VO194) at 20.1 lbs/min using apositive displacement pump.

The centrifuge was spinning at 5138 rpm with an acting force of 5030 g.The outlet ratios were adjusted to 48:52 (light to heavy) by controllingback pressure on the heavy stream to 28 psig and the light phase wasopen to atmosphere or 0 psig. The flow of light stream was measured 9.6lbs/min. and the heavy stream was 10.5 lbs/min. The lights stream solidswere measured at 47.66% and heavies at 4.77%. The inlet slurry had anumber weighted medium particle size of 4.05 microns. The separatedlight phase had a number weighted medium particle size of 10.00 micronsand the heavy phase had a number weighted medium particle size of 1.43microns. The perfume content of the incoming slurry was 20.87%. Theseparated light phase had a perfume content of 44.88% and the heavyphase perfume content was 0.53%. Shell particle removal efficiency was52.9%

The dimensions and values disclosed herein are not to be understood asbeing strictly limited to the exact numerical values recited. Instead,unless otherwise specified, each such dimension is intended to mean boththe recited value and functionally equivalent range surrounding thatvalue. For example, a dimension disclosed as “40 mm” is intended to mean“about 40 mm”.

All documents cited in the Detailed Description of the Invention are, inrelevant part, incorporated herein by reference; the citation of anydocument is not to be construed as an admission that it is prior artwith respect to the present invention. To the extent that any meaning ordefinition of a term in this document conflicts with any meaning ordefinition of the same term in a document incorporated by reference, themeaning or definition assigned to that term in this document shallgovern.

While particular embodiments of the present invention have beenillustrated and described, it would be obvious to those skilled in theart that various other changes and modifications can be made withoutdeparting from the spirit and scope of the invention. It is thereforeintended to cover in the appended claims all such changes andmodifications that are within the scope of this invention.

1. A benefit agent delivery composition comprising, based on totalbenefit agent delivery composition weight: a.) from about 2% to about95% of an encapsulated benefit agent; b.) less than from about 1% toabout 30% shell particles; and c.) the balance of said benefit agentdelivery composition being one or more processing aids and carriers. 2.The benefit agent delivery composition of claim 1, wherein saidencapsulated benefit agent comprises, a benefit agent selected from thegroup consisting of perfumes; brighteners; insect repellants; silicones;waxes; flavors; vitamins; fabric softening agents; skin care agents;enzymes; anti-bacterial agents; bleaches; and mixtures thereof.
 3. Thebenefit agent delivery composition of claim 1, wherein said shellparticles comprises an amino resin.
 4. The benefit agent deliverycomposition of claim 1, wherein said perfume comprises a perfume rawmaterial selected from the group consisting of Quadrant I, II, III andIV perfume raw materials and mixtures thereof.
 5. The benefit agentdelivery composition of claim 1, wherein said one or more processingaids are selected from the group consisting of water, aggregateinhibiting materials, soil suspending polymers, and mixtures thereof. 6.The benefit agent delivery composition of claim 1, wherein said one ormore carriers is selected from the group consisting of polar solvents,nonpolar solvents, and mixtures thereof.
 7. The benefit agent deliverycomposition of claim 6, wherein: a. said perfume comprises a perfume rawmaterial selected from the group consisting of Quadrant I, II, III andIV perfume raw materials and mixtures thereof; b. said one or moreprocessing aids are selected from the group consisting of water,aggregate inhibiting materials, soil suspending polymers, and mixturesthereof; and c. said one or more carriers is selected from the groupconsisting of water, ethylene glycol, propylene glycol, polyethyleneglycol, glycerol, nonpolar solvents, and mixtures thereof. 8-15.(canceled)
 16. A benefit agent delivery composition made by a processcomprising the process of separating shell particles from encapsulatedbenefit agents in a benefit agent delivery composition under conditionssufficient to reduce the percentage of said shell particles in saidbenefit agent delivery composition by at least 20%, said separating stepbeing selected from one or more of centrifuging, filtering, solventexchanging, flash evaporating, decanting, flotation separating, spraydrying, reactive adsorbing, reactive absorbing, and electrophoreticlyseparating, wherein the benefit delivery composition comprises one ormore encapsulated benefit agents and greater than 0.1% shell particles,said shell particles comprising a residual by-product of anencapsulation process.
 21. The benefit agent delivery composition ofclaim 1, wherein said encapsulated benefit agent comprises a sufficientamount of benefit agent to provide, based on total benefit deliverycomposition weight, from about 1% to about 85% benefit agent.
 22. Thebenefit agent delivery composition of claim 2, wherein the skin careagent comprises paraffins.
 23. The benefit agent delivery composition ofclaim 3, wherein the amino resin comprises one or both of a melamineresin and a urea resin.
 24. The benefit agent delivery composition ofclaim 5, wherein the aggregate inhibiting materials comprise divalentsalts.
 25. The benefit agent delivery composition of claim 6, whereinthe polar solvents are selected from the group consisting of water,ethylene glycol, propylene glycol, polyethylene glycol, glycerol, andmixtures thereof.
 26. The benefit agent delivery composition of claim 6wherein the nonpolar solvents are selected from the group consisting ofmineral oil, perfume raw materials, silicone oils, hydrocarbon paraffinoils, and mixtures thereof.
 27. The benefit agent delivery compositionof claim 7 wherein the nonpolar solvents are selected from the groupconsisting of mineral oil, perfume raw materials, silicone oils,hydrocarbon paraffin oils, and mixtures thereof.
 28. The benefit agentdelivery composition of claim 7 wherein the aggregate inhibitingmaterials comprise divalent salts.
 29. The benefit agent deliverycomposition of claim 1 wherein said encapsulated benefit agent comprisesa sufficient amount of benefit agent to provide, based on total benefitdelivery composition weight, from about 1% to about 20% benefit agent.